CN105062405A - LED photocuring non-solvent type photosensitive transfer printing adhesive for cover plate glass substrate and preparation method thereof - Google Patents
LED photocuring non-solvent type photosensitive transfer printing adhesive for cover plate glass substrate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses LED photocuring non-solvent type photosensitive transfer printing adhesive for a cover plate glass substrate. The photosensitive transfer adhesive comprises aliphatic polyurethane acrylate, an acrylate reactive diluent, a photoinitiator, an acrylic auxiliary and a silane coupling agent. The LED photocuring non-solvent type photosensitive transfer printing adhesive for the cover plate glass substrate is free of solvents and environmentally friendly, integrates advantages of the transfer printing technology and advantages of the photosensitive technology, and can be particularly used for development through a pure water neutral developing solution. The LED photocuring non-solvent type photosensitive transfer printing adhesive for the cover plate glass substrate has excellent physical performance, resistant to solvents, resistant to cold and hot impact and good in adhesion with the substrate after being cured. The adhesive force of an adhesive layer and the substrate is larger than 4B and environmental pollution is little especially after a boiling test. The problem that existing UV adhesive is poor in adhesion on cover plate glass and not resistant to boiling or solvents is solved, industrial requirements are met, production cost of enterprises is reduced, and benefits are brought to the enterprises.
Description
Technical field
The present invention relates to photocuring transfer glue technical field, particularly relate to cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue and preparation method thereof.
Background technology
UV transfer glue is generally a kind of single-component ultraviolet curing type glue, mainly through mould molding in material surface, have: easy to use, curing speed is fast, transmittance is high, easy to operate, advantages of environment protection, has been widely used in various plastics film industry.Transfer glue formula generally comprises: active dilution property monomer, light trigger, esters of acrylic acid prepolymer, auxiliary agent etc.UV solidification and ultraviolet light polymerization, UV is ultraviolet english abbreviation.UV solidification refer to utilize in UV-light, shortwave, light trigger in liquid towards raw material carries out radiation, make initiator violent change be free radical or positively charged ion, thus cause the process that the small molecule monomer, resin prepolymer etc. that contain active function groups aggregate into insoluble not molten macromolecular compound.UV solidification is rise a kind of sixties in 20th century, environmental protection, the new technology of basic VOC free discharge.General UV-light refers to the invisible light wave of wavelength within the scope of 0-400nm, and UV solidifies the ultraviolet wavelength that uses generally at 200-400nm.
UV solidification generally refers to condition of cure or the requirement of coating (paint), ink, tackiness agent (glue) or other embedding sealing agent needed with ultraviolet curing, and it is different from heating cure, linking agent (solidifying agent) solidification, spontaneous curing etc.Depend primarily on light trigger and curing process two aspect.The crosslinking reaction speed of resin and the consistency of auxiliary agent also play an important role to a certain extent.The curing mode used now mostly is high pressure mercury arc lamp, the high-pressure halogen lamp that electric power excites, and energy general range is 200-2000i/cm
2, initiator many uses bitter almond oil camphor and derivative, benzil and derivative thereof, methyl phenyl ketone and derivative, acyl group phosphorus compound.
In order to improve the class of goods, the decoration on surface is essential, adopts transfer technique can improve the decoration level of product surface.Tradition UV transfer glue mainly a kind of light-cured type single component single voxel glue, by mould molding in plastic film substrate surfaces such as polycarbonate, polyethylene terephthalate and thermoplastic elastic urethane.Conventional plastic base material is by UV transfer glue when producing in enormous quantities, and often the blocked up problem of excessive glue, thickness appears in material edge, just can ensure very high production yield by the bad part of excision.And cover-plate glass base material is inorganic materials, be different from the organic materialss such as plastics film, once there is the unfavorable conditions such as glue of overflowing, can only scrap, therefore traditional UV glue is difficult to be applied to glass baseplate.
Particularly cover-plate glass is mainly as the touch-screen of high-end electronic product, and added value is very high, often needs special lines, such as CD drawing pattern, AG frosted line etc.For handset touch panel, edge needs special grains to carry out attractive, decorative, and the discreet portions such as touch-screen middle portion and mobile phone front-facing camera must be transparent, thus does not affect mobile phone visual effect and practical application function.And transfer technique can only provide the special grains of full width, can't resolve this specific demand structure of touch-screen.Therefore need, in conjunction with the exposure of photoresists technique, developing process, the part of solidifying will do not needed, use the black film to block, then use developing solution removing uncured portion, retain cured portion, thus reach the specific demand of touch-screen.Heritage optical cement generally can only be developed by organic solvent, or the aqueous solution development of non-neutral, to bad environmental.Therefore need badly and aly can be suitable for the neutral developing solution of water-based, organic solvent developing solution UV colloid system can be suitable for again.The actual production conditions of different manufacturers can be met, be conducive to farthest promoting the environment amenable production technique of the neutral developing liquid developing of water-based simultaneously.
Tradition UV adhesive curing generally adopts environmentally harmful high voltage mercury lamp, high-pressure halogen lamp is cured.In use, heat release is serious in these two kinds of lamp sources, and energy of light source fluctuation is comparatively large, is unfavorable for the volume production stability of UV product.Meanwhile, on this inorganic material of glass, there is particularly outstanding difficulty attachment and the problem of not resistance to boiling water boiling in existing UV glue.And some UV glue products are in order to solve poor adhesion problem on the glass substrate, adding organic solvent, then removing desolventizing by baking process, greatly endangering environment.The technical problem that existing UV glue exists on cover-plate glass base material has 3 points, 1. poor adhesive force on cover-plate glass base material.2. resistance to boiling water boiling poor performance on cover-plate glass base material.3. most UV colloid system is containing organic solvent, inflammable and explosive, harm environment.4. environmentally harmful high voltage mercury lamp, high-pressure halogen lamp is used to solidify.5. can not meet the special grains requirement of cover-plate glass, full width solidification can only be carried out, can not local solidification.7. visualization way is single, and glue can not develop in the neutral developing solution of pure water.Therefore, the no-solvent type sensitive transfer glue of a kind of novel cover-plate glass base material for high added value of necessary research and development, not only solves the application performance of transfer glue, can also be suitable for LED light solidification, and environmental protection.
Summary of the invention
The object of this invention is to provide a kind of no-solvent type sensitive transfer glue of LED light solidification of the novel cover-plate glass base material for high added value; It is not containing solvent, and environmental friendliness, in conjunction with transfer printing and photosensitive technological advantage, design is unique, and composition is rationally, easy to prepare, solve the requirement of cover-plate glass base material special grains, on cover-plate glass base material, sticking power is excellent simultaneously, improves the resistance to boiling water boiling performance on cover-plate glass material; The neutral developing solution of water-based or organic solvent developing liquid developing can be used, pure water particularly can be used to develop, accomplish the real environmental sound of developing solution, nontoxic, do not fire not quick-fried, and no matter use which kind of visualization way above-mentioned, development effect is very good, and clear without cull, lines, figure is accurate, attractive in appearance.Not only expanded the Application Areas of transfer glue on cover-plate glass class inorganic substrate, the simultaneously compatible advantage of photoresists technique and UV transfer glue technique, solves the problem that existing transfer glue can only be applied to organic film substantially.
For achieving the above object, the technical solution used in the present invention is:
A kind of cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue, by weight, composed of the following components:
In the present invention, aliphatic polyurethane CALCIUM ACRYLATE is one or more in hydroxyl modification bifunctional fat adoption ammonia ester acrylate, carboxy-modified trifunctional aliphatic urethane acrylate, six functional groups aliphatic urethane acrylate.The carboxyl acid modified trifunctional aliphatic urethane acrylate UV4900 of such as Shenzhen ComeOn brightness Chemical Industry Science Co., Ltd; The hydroxyl modification two of the good photochemical Science and Technology Ltd. of Shenzhen ancient cooking vessel can roll into a ball aliphatic urethane acrylate DH-305; The carboxy-modified aliphatic urethane acrylate 5652 of hydroxyl modification trifunctional of Tianjin glycolylurea Ci Co., Ltd; The bifunctional hydroxyl modification two of Changxing company limited can roll into a ball aliphatic urethane acrylate DU-U153, six functional groups aliphatic urethane acrylate 6146-100; The six functional groups group aliphatic polyurethane CN9010NS etc. of Sartomer.Resin is the major embodiment person of glue performance, it not only coordinates the function of each component in glue system, make between each component, to play collaborative promoter action, avoid the defect that a certain component brings overall performance to decline, self mainly bear the fundamental propertys such as bonding, cold-hot after film-forming impact, weather-proof, resistance to chemical attack simultaneously.More importantly resin system composition of the present invention rationally, makes the harmonious organic whole that glue System forming is unified.Aliphatic urethane acrylate has the advantage such as reactive behavior and functional group that toughness is good, shrinking percentage is low, higher, aliphatic urethane acrylate particularly after percarboxylic acids or hydroxyl modification and the polarity of glass baseplate close, certain sticking power can be had with glass baseplate, also there is the performance of the chemical corrosions such as ethanol-tolerant; Meanwhile, introduce hydrophilic carboxyl, hydroxyl polar group, be also beneficial to by the neutral developing liquid developing of pure water.Solve the difficult attachment issue of glue on cover-plate glass base material, improve the resistance to chemical attack such as water boiling resistance and ethanol-tolerant problem, improve washing developing liquid developing ability, thus take into account water-based and solvent-borne type and to develop two kinds of modes.
In the present invention, acrylated phosphate compounds is one or more in methacrylic acid phosphoric acid ester, 2-hydroxyethyl methacrylic acid phosphoric acid ester, methylacryoyloxyethyl phosphoric acid ester; Preferred 2-hydroxyethyl methacrylic acid phosphoric acid ester; High acid value acrylate analog assistant of the present invention is with abundant polar group, reactive strong, when glue curing, the carbon-carbon double bond that acrylate analog assistant contains itself participates in curing reaction, simultaneously with polar group can with the siloxane bond generation chemical reaction in the inorganic substrate such as glass, form very large reactive force, effectively add the sticking power of glue and glass baseplate, solve existing glue and cannot form the difficult problem of strong reactive force with inorganic substrate.And polar group is also conducive to pure water development, thus takes into account water-based and solvent-borne type and to develop two kinds of modes.
In the present invention, esters of acrylic acid reactive monomer is 2-Hydroxy ethyl acrylate, iso-bornyl acrylate, 2-hydroxypropyl acrylate, ethoxyquin Viscoat 295,1,6-hexanediyl ester, 1, one or more in 4-hexanediyl ester, 1,4 butanediol diacrylate, dipentaerythritol acrylate.Reactive monomer can regulation system viscosity, makes each component disperses even, increases the interface synergy between each component, thus obtain the glue of high comprehensive performance.Simultaneously as the thinner with active group, such as its hydroxy functional group of 2-Hydroxy ethyl acrylate and resin body the chemical bond with the inorganic substrate such as polar group and glass (siloxane bond of such as its inside) chemical bond power can be formed, significantly increase the sticking power of transfer glue and base material.
In the present invention; light trigger is 2-hydroxyl-2 methyl isophthalic acid phenyl-1-acetone, benzoin dimethylether, phenyl two (2; 4; 6-trimethylbenzoyl) phosphine oxide, 2; one or more in 4,6-trimethylbenzoy-dipheny phosphine oxide, 1-hydroxy-cyclohexyl-phenyl ketone, benzophenone, 2-methyl isophthalic acid-[4-(methylthio group) phenyl]-2-morpholinyl-1-acetone.The LED Spectral matching of 365nm wavelength fixed by light trigger and cold light source, at utmost plays photoinitiation, fully can absorb light source, and produce radical crosslinking reaction, glue is solidified completely, ensures its performance.
In the present invention, silane coupling agent is one or more in vinyltrimethoxy silane, vinyltrimethoxy silane, triethoxy methyl silicane, 3-methacrylic acid propyl group three (trimethyl silane).Coupling agent consumption is less, but it can increase and cover-plate glass substrate interface reactive force in glue system, as the gap filling up macromolecular compound interchain as trying to make a match, effectively improves the water boiling resistance performance after transfer glue solidification.
In the present invention, LED light wavelength is 365nm.The LED of fixed wave length, environmental friendliness, not heat release substantially, energy is highly stable, solves existing curing mode heat release serious, and energy of light source fluctuation is comparatively large, is unfavorable for the problem of product volume production stability.
Preferably, by weight, described cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue is composed of the following components:
The invention also discloses the preparation method of above-mentioned cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue, comprise the following steps:
(1) 80-90% of aliphatic polyurethane CALCIUM ACRYLATE, esters of acrylic acid reactive monomer total mass, light trigger and acrylate phosphate compounds are added successively in container, mixing, dispersion, filtration, obtain host;
(2) residual acrylic acid ester class activity diluting monomer, silane coupling agent are added in container successively and mixed, dispersion, filtration, obtain assistant agent;
(3) 10: 1 mixing hosts and assistant agents in mass ratio, dispersion, filter, and namely obtain cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue.
In above-mentioned steps (1), dispersion rate is that 1000-1500 turns/min, and the time is 1-4 hour; In step (2), dispersion rate is that 200-500 turns/min, and the time is 0.5-1 hour; In step (3), dispersion rate is that 200-500 turns/min, and the time is 0.5-1 hour; In step (1), step (2) and step (3), the environment of dispersion is lucifuge, ventilated environment, and temperature is 15-35 DEG C.
Above-mentioned cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue can be applicable to cover-plate glass base material transfer process, comprises the following steps: be coated with described cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue at cover-plate glass substrate surface; And then cover film diaphragm; Then LED light source 100-200mJ/cm is used
2low-yield Procuring exposure; Then remove film diaphragm, use the not photosensitive part glue of developing solution dissolution; Then dry up or dry residual developing solution; Finally use LED light source 1000-2000mJ/cm
2transfer glue after the development of high-energy regelate, namely completes the transfer process of cover-plate glass base material; Described developing solution is water or organic solvent type developing solution; Be preferably water.
Wherein pure water developing solution is non-combustible, without organism volatilization, non-explosive; Organic solvent developing solution is made up of one or more in ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol or Pentyl alcohol.
Can be there is series of physical, chemical transformation in glue, these change and the character of glue itself, add the difference of construction parameter in construction and film process, may the application performance of remarkably influenced glue.Such as, after glue application, there will be new interface, if the interfacial tension of the liquid/liquid/solid interface between glue and material is higher than the critical surface tension of material, glue just cannot be sprawled smoothly on material, can produce the bad defect such as flake, shrinkage cavity; During solvent-laden adhesive curing, because of curing exotherm, the volatilization of solvent can be promoted, will cause between film surface and inside, produce temperature, density and surface tension poor, these differences and then cause producing the turbulent motion of glued membrane inside, form so-called vortex, vortex can cause producing the bad phenomenon such as tangerine peel; In curing system, not only there is a kind of resin, just may produce insoluble micelle at solidification process, cause surface tension gradient to be formed.Activity diluting monomer, resin oligomers, each analog assistant in special glue composition, all may there is the situation of carrying and enriching reactive group, reactive uncertain between macromolecule resin oligopolymer, small molecule active diluting monomer, auxiliary agent, glue is at preparation, solidification process, all there is multiple reaction, this situation can cause glue to be coated in material surface, and after solidification, every physics, the chemical property of glue are unstable.
The invention devise new glue system, resin and additive, particularly with active group all the other compounds between consistency good, and the component producing adverse chemical reaction separately stores, and ensures the stability in storage of glue.And glue can not produce side reaction when preparing and solidify between organism substantially, ensureing the reactive behavior on glue and cover-plate glass material surface, improving the interface interaction power of glue and material, effectively improve the bonding force of glue/material.Glue system stability is good, not perishable, and after storage, when temperature-resistant, viscosity does not change substantially; During solidification, reactivity is good, and double bond conversion rate is high, and coating performance is good; After glue curing, the corrosive powers such as ethanol-tolerant are strong, and the weathering resistance had, and long-time nondiscoloration, fade; Not easily xanthochromia.Cured glue layer has excellent bonding force to material, solves the problem of glue difficult attachment on the inorganic substrates such as cover-plate glass.
In addition, prior art, in order to improve the interfacial effect of glue and base material, reduces above-mentioned defect as far as possible, can to base material pre-treatment before glue application; The cleaning of thorough guarantee base material.Glue is directly constructed by newly-designed sensitive transfer process by the present invention, glue-line after solidification and substrate bonding good, without boundary defect, the special lines that ensure that product require with outward appearance while, effectively improve the resistance to chemical attack ability such as water boiling resistance and ethanol-tolerant of base material.
Because technique scheme is used, the present invention compared with prior art has following advantages:
1. the cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue that the present invention is first public, design is unique, composition rationally, easy to prepare, have excellent in base material sticking power, while raising glue cementability performance, in turn ensure that the lines appearance requirement that cover-plate glass is special, improve water boiling resistance, chemical resistance, simultaneously environmentally friendly.
2. cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue disclosed by the invention only needs very thin glue-line, only need 6-10 micron, still achieve excellent cementability and water boiling resistance, chemical resistance, boiling water boiling 10 minutes, film surface is as good as shape, sticking power is still greater than 4B, overcomes the defect that the thicker glue-line of existing needs still can not improve chemical resistance, water boiling resistance, achieves beyond thought technique effect.
3. cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue provided by the invention is by the LED solidification of fixing 365nm wavelength, environmental friendliness, not heat release substantially, energy stabilization, abandon environmentally harmful, the obvious high voltage mercury lamp of shortcoming, high-pressure halogen lamp.
4. cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue provided by the invention is not containing solvent, but each component compatibility is good, between organism, Harmony is good, without aggregation phenomenon, avoids the defect of the glued membrane overall performance decline that the outstanding relative merits of a certain component self are brought; Simultaneously under the effect of each reactive group synergistic effect, resin system solidification effect is good, obtain certain heat-resisting, chemically-resistant, mechanical property improves, special organism and mineral surfaces react, interface interaction power is high, thus obtains the glued membrane of the excellent combination properties such as sticking power, rub resistance, solvent resistant, weathering resistance.
5. the invention acrylate analog assistant, esters of acrylic acid reactive monomer, silane coupling agent are added in aliphatic urethane acrylate, add successively, each component supplements and complements each other, and maximizes favourable factors and minimizes unfavourable ones, and can separately store by reactive component; Polar group that each component is with can increase respective intermolecular forces simultaneously, but can not overreaction, ensure the reactivity of organic-compound system and inorganic substrate, thus while raising glue and material sticking power, the glued membrane after solidification still has excellent over-all properties.
6. cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue provided by the invention uses and stores conveniently, and under the prerequisite meeting high bonding requirements, only need once be coated with, thickness is thin, consumption is few, friendly to the pollution of environment, lower to the injury of human body; And because resin composition is reasonable, glue curing reactivity is good, the glue-line good combination property after solidification, the neutral developing solution of pure water or solvent-borne type developing liquid developing can be used, be more suitable for suitability for industrialized production.Particularly pure water development, this kind of visualization way environmental sound is the main flow that futurity industryization is produced.
Accompanying drawing explanation
Fig. 1 is the photo figure before and after the test of embodiment one product sticking power;
Fig. 2 is outside drawing before and after embodiment two product 150 DEG C baking;
Fig. 3 is the photo figure before and after the resistance to ethyl acetate test of embodiment three products;
Fig. 4 is the photo figure before and after the hot and humid test of embodiment four-product;
Fig. 5 is the photo figure before and after the test of embodiment five product thermal shock.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
Embodiment one
By weight, by carboxy-modified for the hydroxyl modification trifunctional of 40 parts of Tianjin glycolylurea Ci Co., Ltd aliphatic urethane acrylate 5652, the carboxyl acid modified trifunctional aliphatic urethane acrylate UV4900 of 10 parts of Shenzhen ComeOn brightness Chemical Industry Science Co., Ltd, 41 parts of iso-bornyl acrylate reactive monomers, 1 part of phenyl two (2, 4, 6-trimethylbenzoyl) phosphine oxide, 1 part 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide, 2 parts of benzophenone, 5 parts of HEMA phosphate adjuvant add in stirring dispersion machine successively, normal pressure, 25 DEG C, lucifuge, dry, ventilated environment, stir 4 hours in 1000 revs/min, dispersed with stirring is even, filter clean impurity, lucifuge, pack, for host,
By weight, by 3 parts of iso-bornyl acrylates, 2 part 1,6-hexanediyl ester, 2 parts of vinyltrimethoxy silanes, 3 parts of 3-methacrylic acid propyl group three (trimethyl silane) add in stirring dispersion machine successively, normal pressure, 25 DEG C, lucifuge, drying, ventilated environment, stir 0.5 hour in 500 revs/min, dispersed with stirring is even, filters clean impurity, lucifuge, packing, is assistant agent;
Get above-mentioned host and assistant agent respectively, mass ratio is 10: 1, add successively in stirring dispersion machine, normal pressure, 35 DEG C, lucifuge, drying, ventilated environment, stir 1 hour in 400 revs/min, dispersed with stirring is even, filters clean impurity, namely obtains cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue.
Embodiment two
By weight, by carboxy-modified for the hydroxyl modification trifunctional of 40 parts of Tianjin glycolylurea Ci Co., Ltd aliphatic urethane acrylate 5652, 41 parts of iso-bornyl acrylates, the six functional groups aliphatic polyurethane CALCIUM ACRYLATE CN9010NS of 10 parts of Sartomer, 2 part 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide, 2 parts of benzophenone, 5 parts of HEMA phosphate adjuvant add in stirring dispersion machine successively, normal pressure, 35 DEG C, lucifuge, dry, ventilated environment, stir 4 hours in 1000 revs/min, dispersed with stirring is even, filter clean impurity, lucifuge, pack, for host,
By weight, by 3 parts of 2-Hydroxy ethyl acrylates, 2 part 1,6-hexylene glycol and acrylate, 2 parts of vinyltrimethoxy silanes, 3 parts of triethoxy methyl silicanes add in stirring dispersion machine successively, normal pressure, 25 DEG C, lucifuge, drying, ventilated environment, stir 0.5 hour in 500 revs/min, dispersed with stirring is even, filters clean impurity, lucifuge, packing, is assistant agent;
Get above-mentioned host and assistant agent respectively, mass ratio is 10: 1, add successively in stirring dispersion machine, normal pressure, 25 DEG C, lucifuge, drying, ventilated environment, stir 0.8 hour in 300 revs/min, dispersed with stirring is even, filters clean impurity, i.e. cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue.
Embodiment three
By weight, by carboxy-modified for the hydroxyl modification trifunctional of 45 parts of Tianjin glycolylurea Ci Co., Ltd aliphatic urethane acrylate 5652, the six functional groups aliphatic urethane acrylate 6146-100 of 5 parts of Changxing company limiteds, 41 parts of iso-bornyl acrylate reactive monomers, 2 part 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide, 2 parts of 1-hydroxy-cyclohexyl-phenyl ketones, 5 parts of HEMA phosphate adjuvant add in stirring dispersion machine successively, normal pressure, 25 DEG C, lucifuge, dry, ventilated environment, stir 4 hours in 1000 revs/min, dispersed with stirring is even, filter clean impurity, lucifuge, pack, for host,
By weight, 2 parts of vinyltrimethoxy silanes, 3 parts of triethoxy methyl silicanes, 5 parts of 2-hydroxypropyl acrylates are added in stirring dispersion machine successively, normal pressure, 25 DEG C, lucifuge, drying, ventilated environment, stir 1 hour in 500 revs/min, dispersed with stirring is even, filtering clean impurity, lucifuge, to pack, is assistant agent;
Get above-mentioned host and assistant agent respectively, mass ratio is 10: 1, add successively in stirring dispersion machine, normal pressure, 25 DEG C, lucifuge, drying, ventilated environment, stir 0.8 hour in 300 revs/min, dispersed with stirring is even, filters clean impurity, namely obtains cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue.
Embodiment four
By weight, by carboxy-modified for the hydroxyl modification trifunctional of 30 parts of Tianjin glycolylurea Ci Co., Ltd aliphatic urethane acrylate 5652, the hydroxyl modification two of 15 parts of good photochemical Science and Technology Ltd.s of Shenzhen ancient cooking vessel can roll into a ball aliphatic urethane acrylate DH-305, the six functional groups aliphatic polyurethane CALCIUM ACRYLATE CN9010NS of 5 parts of Sartomer, 35 parts of iso-bornyl acrylate reactive monomers, 6 parts of 2-Hydroxy ethyl acrylates, 2 part 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide, 2 parts of 1-hydroxy-cyclohexyl-phenyl ketones, 5 parts of HEMA phosphate adjuvant add in stirring dispersion machine successively, normal pressure, 25 DEG C, lucifuge, dry, ventilated environment, stir 4 hours in 1000 revs/min, dispersed with stirring is even, filter clean impurity, lucifuge, pack, for host,
By weight, 2 parts of vinyltrimethoxy silanes, 3 parts of triethoxy methyl silicanes, ethoxyquin Viscoat 295s are added in stirring dispersion machine successively, normal pressure, 25 DEG C, lucifuge, drying, ventilated environment, stir 1 hour in 500 revs/min, dispersed with stirring is even, filtering clean impurity, lucifuge, to pack, is assistant agent;
Get above-mentioned host and assistant agent respectively, mass ratio is 10: 1, add successively in stirring dispersion machine, normal pressure, 25 DEG C, lucifuge, drying, ventilated environment, stir 0.8 hour in 300 revs/min, dispersed with stirring is even, filters clean impurity, namely obtains cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue.
Embodiment five
By weight, by carboxy-modified for the hydroxyl modification trifunctional of 35 parts of Tianjin glycolylurea Ci Co., Ltd aliphatic urethane acrylate 5652, the bifunctional hydroxyl modification two of 10 parts of Changxing company limiteds can roll into a ball aliphatic urethane acrylate DU-U1535 part, the six functional groups aliphatic polyurethane CALCIUM ACRYLATE CN9010NS of 5 parts of Sartomer, 36 parts of iso-bornyl acrylate reactive monomers, 5 parts of ethoxyquin Viscoat 295s, 2 part 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide, 2 parts of 1-hydroxy-cyclohexyl-phenyl ketones, 5 parts of HEMA phosphate adjuvant add in stirring dispersion machine successively, normal pressure, 25 DEG C, lucifuge, dry, ventilated environment, stir 4 hours in 1000 revs/min, dispersed with stirring is even, filter clean impurity, lucifuge, pack, for host,
By weight, 2 parts of vinyltrimethoxy silanes, 3 parts of 3-methacrylic acid propyl group three (trimethyl silane), ethoxyquin Viscoat 295,3 parts of 2-Hydroxy ethyl acrylates are added in stirring dispersion machine successively, normal pressure, 25 DEG C, lucifuge, drying, ventilated environment, stir 1 hour in 500 revs/min, dispersed with stirring is even, filtering clean impurity, lucifuge, to pack, is assistant agent;
Get above-mentioned host and assistant agent respectively, mass ratio is 10: 1, add successively in stirring dispersion machine, normal pressure, 25 DEG C, lucifuge, drying, ventilated environment, stir 0.8 hour in 300 revs/min, dispersed with stirring is even, filters clean impurity, namely obtains cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue.
Above-mentioned cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue is carried out following technique to glass baseplate transfer process:
1, embodiment one to four adopts pure water neutral developing liquid developing mode technique:
Glue is coated cover-plate glass material surface; Cover containing the film diaphragm of grain pattern, film diaphragm has can exposure area and black occlusion area; By rubber roll by film diaphragm, glue, the tight pressing of material; The LED of fixing 365nm wavelength is used to carry out Procuring exposure, Procuring energy: 100-200mJ/cm
2; Throw off film diaphragm, then developed by pure water; Baking drying adhesive layer surface development liquid, baking condition: 85-95 DEG C of baking 15min; Regelate, profound solidification energy: 1000-2000mJ/cm
2, the performance test such as physics, chemistry is carried out to glue-line.
2, embodiment five adopts solvent-borne type developing liquid developing mode technique:
Glue is coated cover-plate glass material surface; Cover containing the film diaphragm of special grains pattern, film diaphragm has can exposure area and black occlusion area; By rubber roll by film diaphragm, glue, the tight pressing of material; The LED of 365nm wavelength is used to carry out Procuring exposure, Procuring energy: 180mJ/cm
2; Throw off film diaphragm, the solvent-borne type developing liquid developing then by being made up of equal-volume ethanol, n-propyl alcohol, Virahol, propyl carbinol, isopropylcarbinol, Pentyl alcohol; Spray gun is used to dry up film surface developing solution, processing condition: 28 DEG C, the spray gun of 1.1MPA pressure blows 8min; Regelate, profound solidification energy: 1800mJ/cm
2, the performance test such as physics, chemistry is carried out to glue-line.
Following items test is carried out to above-mentioned cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue: thickness, film thickness gauge; Outward appearance, range estimation and 60 times of magnifying glasses; Hardness, handcard type pencil hardometer, load 750g; After after ethanol-tolerant, embodiment glue curing, normal temperature places 24 hours, glue is placed in ventilation, cool place, 25 DEG C of environment spirituous solution soak 10min; After after resistance to ethyl acetate, glue curing, normal temperature places 24 hours, glue is placed in ventilation, cool place, 25 DEG C of environment ethyl acetate solution soak 10min; After normal temperature places 24 hours after high-temp resisting high-humidity resisting, glue curing, be placed in temperature 85 DEG C, place 72 hours under humidity 85% environment; The square small grid of 10 × 10 1mm × 1mm is drawn in sticking power test, the film surface of use sharp cutter (knife edge angle 15 ~ 30 °) after embodiment solidification, and every bar is rule deeply and glue-line bottom, touches glass surface.Use banister brush by clean for the fragment of test zone clean, then 3M company No. 600 adhesive tapes (adhesive power 300 ~ 400g/cm2) is used firmly to cling net region 30 seconds, catch adhesive tape one end with hand, (90 °) shut down adhesive tape rapidly in the vertical direction.Same position, same method tests 3 times; After cold-hot impacts, normal temperature places 24 hours after glue curing, first place-16 DEG C of environment and keep 30min, be then rapidly heated to 80 DEG C and keep 30min to be 1 circulation, totally 10 circulations; After normal temperature places 24 hours after water boiling resistance, embodiment glue curing, put into 100 DEG C of thermostat water bath 10min, then leave standstill and dry 0.5 hour, ensure that glue-line is dry;-16 DEG C of environment are positioned over after low temperature resistant, embodiment glue curing; 150 DEG C of baking 30min are carried out after high temperature resistant, embodiment glue curing; After carrying out 150 DEG C of baking 30min after high temperature after water boiling resistance performance, embodiment glue curing, put into 100 DEG C of thermostat water bath 30min, then use non-dust cloth wipe surfaces, dry standing 3-5min.
After the adhesive curing of above-mentioned cover-plate glass base material LED light solidification no-solvent type sensitive transfer, test result is as table 1.
Table 1 test result
Accompanying drawing 1 is the photo figure before and after the test of embodiment one product sticking power, can finding out, being judged to be 5B according to the invention provides sticking power testing standard.
Accompanying drawing 2 is outside drawing before and after embodiment two product 150 DEG C baking, can find out, outward appearance not now considerable change before and after baking.
Accompanying drawing 3 is the photo figure before and after the resistance to ethyl acetate test of embodiment three products, can obviously find out, the resistance to ethyl acetate test of transfer glue prepared according to the methods of the invention does not show abnormal appearance.
Accompanying drawing 4 is the photo figure before and after the hot and humid test of embodiment four-product, can obviously find out, after the hot and humid test of transfer glue prepared according to the methods of the invention, does not show abnormal appearance.
Accompanying drawing 5 is the photo figure before and after the test of embodiment five product thermal shock, can obviously find out, after transfer glue thermal shock prepared according to the methods of the invention, does not show abnormal appearance.
According to the cover-plate glass base material figure after above-mentioned transfer glue process, can find out: because cover-plate glass cannot cut, therefore product of the present invention solves cover-plate glass and to overflow glue problem, simultaneously, the front-facing camera hole on such as front glass top, do not need glue to cover, product of the present invention also solves this problem smoothly; And each hole very circle on cover-plate glass, and cover without glue.
Claims (10)
1. a cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue, is characterized in that: by weight, and described cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue is composed of the following components:
2. cover-plate glass base material LED light solidifies no-solvent type sensitive transfer glue according to claim 1, it is characterized in that: described aliphatic polyurethane CALCIUM ACRYLATE is one or more in hydroxyl modification bifunctional fat adoption ammonia ester acrylate, carboxy-modified trifunctional aliphatic urethane acrylate, six functional groups aliphatic urethane acrylate.
3. cover-plate glass base material LED light solidifies no-solvent type sensitive transfer glue according to claim 1, it is characterized in that: described acrylated phosphate compounds is one or more in methacrylic acid phosphoric acid ester, 2-hydroxyethyl methacrylic acid phosphoric acid ester, methylacryoyloxyethyl phosphoric acid ester.
4. cover-plate glass base material LED light solidifies no-solvent type sensitive transfer glue according to claim 1, it is characterized in that: described esters of acrylic acid reactive monomer is 2-Hydroxy ethyl acrylate, iso-bornyl acrylate, 2-hydroxypropyl acrylate, ethoxyquin Viscoat 295,1,6-hexanediyl ester, 1, one or more in 4-hexanediyl ester, 1,4 butanediol diacrylate, dipentaerythritol acrylate.
5. cover-plate glass base material LED light solidifies no-solvent type sensitive transfer glue according to claim 1; it is characterized in that: described light trigger is 2-hydroxyl-2 methyl isophthalic acid phenyl-1-acetone, benzoin dimethylether, phenyl two (2; 4; 6-trimethylbenzoyl) phosphine oxide, 2; one or more in 4,6-trimethylbenzoy-dipheny phosphine oxide, 1-hydroxy-cyclohexyl-phenyl ketone, benzophenone, 2-methyl isophthalic acid-[4-(methylthio group) phenyl]-2-morpholinyl-1-acetone.
6. cover-plate glass base material LED light solidifies no-solvent type sensitive transfer glue according to claim 1, it is characterized in that: described silane coupling agent is one or more in vinyltrimethoxy silane, triethoxy methyl silicane, vinyltrimethoxy silane, 3-methacrylic acid propyl group three (trimethyl silane).
7. cover-plate glass base material LED light solidifies no-solvent type sensitive transfer glue according to claim 1, it is characterized in that, by weight, described cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue is composed of the following components:
8. the preparation method of LED light solidification no-solvent type sensitive transfer glue of any one cover-plate glass base material described in claim 1-7, is characterized in that, comprise the following steps:
(1) 80-90% of aliphatic polyurethane CALCIUM ACRYLATE, esters of acrylic acid reactive monomer total mass, light trigger and acrylate phosphate compounds are added successively in container, mixing, dispersion, filtration, obtain host;
(2) residual acrylic acid ester class activity diluting monomer, silane coupling agent are added in container successively and mixed, dispersion, filtration, obtain assistant agent;
(3) 10: 1 mixing hosts and assistant agents in mass ratio, dispersion, filter, and namely obtain cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue.
9. cover-plate glass base material solidifies the preparation method of no-solvent type sensitive transfer glue by LED light according to claim 8, and it is characterized in that: in step (1), dispersion rate is that 1000-1500 turns/min, and the time is 1-4 hour; In step (2), dispersion rate is that 200-500 turns/min, and the time is 0.5-1 hour; In step (3), dispersion rate is that 200-500 turns/min, and the time is 0.5-1 hour; In step (1), step (2) and step (3), the environment of dispersion is lucifuge, ventilated environment, and temperature is 15-35 DEG C.
10. the application of LED light solidification no-solvent type sensitive transfer glue in cover-plate glass base material transfer process of any one cover-plate glass base material described in claim 1-7, is characterized in that: during described transfer process, developing solution is water.
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