CN105062405B - Cover-plate glass base material cures no-solvent type sensitive transfer glue and preparation method thereof with LED light - Google Patents
Cover-plate glass base material cures no-solvent type sensitive transfer glue and preparation method thereof with LED light Download PDFInfo
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Abstract
The invention discloses a kind of cover-plate glass base material LED lights to cure no-solvent type sensitive transfer glue, including aliphatic polyurethane acrylate, esters of acrylic acid reactive diluent, photoinitiator, acrylate analog assistant, silane coupling agent.The cover-plate glass base material of the present invention is solvent-free with LED light solidification no-solvent type sensitive transfer, environmental-friendly, takes into account the advantages of transferring with photosensitive two kinds of technique, can especially use pure water neutrality developing liquid developing.The cover-plate glass base material of present invention LED light has excellent physical property, solvent resistant, cold-resistant thermal shock and glue-line and substrate bonding good after curing no-solvent type sensitive transfer adhesive curing, especially after boiling test, still ＞ 4B, environmental pollution are small for the adhesive force of glue-line and base material.It solves the problems, such as that existing UV glue cementability on cover-plate glass is poor, not water boiling resistance, not solvent resistant, meets industry requirement, reduce enterprise's production cost, be enterprise getting profit.
Description
Technical field
It is solvent-free with LED light solidification that the present invention relates to photocuring transfer glue technical fields more particularly to cover-plate glass base material
Type sensitive transfer glue and preparation method thereof.
Background technology
UV transfer glues are usually a kind of one-component ultraviolet curing type glue, are mainly molded in material surface,
Have：It is easy to use, curing rate is fast, light transmittance is high, easy to operate, advantages of environment protection, have been widely used for various
Plastic film industry.Transfer glue formula generally comprises：Active diluent monomers, photoinitiator, esters of acrylic acid prepolymer, auxiliary agent
Deng.UV solidifications are ultraviolet light solidification, and UV is the english abbreviation of ultraviolet light.UV solidifications refer to using in ultraviolet light, shortwave, to liquid
Photoinitiator in state raw material is radiated, and it is free radical or cation to make initiator violent change, contains active function groups to cause
Small molecule monomer, resin prepolymer etc. aggregate into the process of insoluble insoluble high-molecular compound.UV solidifications are a kind of 20 generation
The new technology that VOC free that the sixties rises, environmentally friendly, basic of recording discharges.General ultraviolet light refers to wavelength in 0-400nm ranges
Interior invisible light wave, the used ultraviolet wavelength of UV solidifications is generally in 200-400nm.
UV solidifications generally refer to need coating (paint), ink, adhesive (glue) or the other fillings with ultraviolet curing
Condition of cure or the requirement for sealing sealant, are different from heating cure, crosslinking agent (curing agent) solidification, spontaneous curing etc..Mainly
Depending on two aspect of photoinitiator and curing process.The cross-linking reaction speed of resin and the compatibility of auxiliary agent are to a certain extent
It plays an important role.Curing mode used today is mostly the high pressure mercury arc lamp of electric power excitation, high-pressure halogen lamp, the general model of energy
It is 200-2000i/cm to enclose2, initiator mostly using benzoin and its derivative, benzil and its derivative, acetophenone and its spreads out
Biology, acyl group phosphorus compound.
In order to improve the class of product, the decoration on surface is essential, and product surface can be improved using transfer technique
Decoration is horizontal.Traditional UV transfer glues are mainly a kind of molding dispensing of light-cured type one pack system, be molded in makrolon,
The plastic film substrates such as polyethylene terephthalate and thermoplastic elastic polyurethane surface.Conventional plastic base material is transferred with UV
For glue when producing in enormous quantities, often there is the blocked up problem of excessive glue, film thickness in material edge, can be protected by cutting off bad part
The very high production yield of card.And cover-plate glass base material is inorganic material, is different from the organic materials such as plastic film, once it overflows
A problem that glue, can only scrap, therefore tradition UV glue is difficult to apply to glass baseplate.
Especially for cover-plate glass mainly as the touch screen of high-end electronic product, added value is very high, and it is special to generally require
Lines, such as CD drawing patterns, AG frosted lines etc..By taking handset touch panel as an example, edge needs special grains to carry out beautiful dress
Decorations, and the discreet portions such as touch screen middle section and mobile phone front camera must be transparent, to not influence mobile phone visual effect
With practical application function.And transfer technique can only provide the special grains of full width, can't resolve this specific demand knot of touch screen
Structure.Therefore the exposure in conjunction with photosensitive adhesive process, developing process are needed, cured part will not needed, blocked using the black film,
Then it uses developer solution to remove uncured portion, retains cured portion, to reach the specific demand of touch screen.Traditional photoresists
It can only generally be developed by organic solvent or the aqueous solution of non-neutral develops, it is harmful to environment.Therefore there is an urgent need for it is a can
It is applicable in water-based neutrality developer solution, and organic solvent developer solution UV colloids system can be applicable in.The practical life of different manufacturers can be met
Production condition, while being conducive to promote the environment amenable production technology of water-based neutrality developing liquid developing to the greatest extent.
Traditional UV adhesive curings are generally cured using environmentally harmful high-pressure sodium lamp, high-pressure halogen lamp.Both lamps
In use, heat release is serious in source, and energy of light source fluctuation is larger, is unfavorable for the volume production stability of UV products.Meanwhile it is existing
There is especially prominent difficult attachment and intolerant to boiling water boiling on this inorganic material of glass in UV glue.And some UV glue
Product is added organic solvent, then removes solvent by baking process, greatly to solve the problems, such as poor adhesion on the glass substrate
Endanger environment greatly.Existing UV glue has at 3 points in technical problem present on cover-plate glass base material, 1. on cover-plate glass base material
Poor adhesive force.2. the resistance to boiling water boiling poor performance on cover-plate glass base material.3. majority UV colloids system contains organic solvent, inflammable and explosive,
Endanger environment.4. being cured using environmentally harmful high-pressure sodium lamp, high-pressure halogen lamp.5. can not meet the special line of cover-plate glass
Road requires, and can only carry out full width solidification, be unable to local solidification.7. visualization way is single, glue cannot be in pure water neutrality developer solution
Middle development.Therefore, it is necessary to research and develop a kind of photosensitive turn of no-solvent type of the novel cover-plate glass base material for high added value
Glue is printed, the application performance of transfer glue is not only solved, moreover it is possible to be applicable in LED light solidification, and environmental protection.
Invention content
The object of the present invention is to provide a kind of cured nothings of LED light of the novel cover-plate glass base material for high added value
Solvent type sensitive transfer glue；It is free of solvent, environmental-friendly, and in conjunction with transfer and photosensitive technological advantage, design is unique, and composition closes
Reason, it is convenient to prepare, and solves the requirement of cover-plate glass base material special grains, while adhesive force is excellent on cover-plate glass base material,
Improve the resistance to boiling water boiling performance on cover-plate glass material；Water-based neutrality developer solution or organic solvent developer solution can be used aobvious
Shadow can especially be developed using pure water, accomplish the real environmental sound of developer solution, nontoxic, non-ignitable not quick-fried, and no matter be made
With which kind of above-mentioned visualization way, development effect is very good, and no residue glue, lines are clear, and figure is accurate, beautiful.It has not only expanded turn
Application field of the glue on cover-plate glass class inorganic substrate is printed, while being compatible with the excellent of photosensitive adhesive process and UV transfer adhesive process
Point solves the problems, such as that existing transfer glue can be only applied to organic film substantially.
In order to achieve the above objectives, the technical solution adopted by the present invention is：
A kind of cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue, by weight, by following components group
At：
In the present invention, aliphatic polyurethane acrylate be hydroxyl modification difunctional fat adoption urethane acrylate,
Carboxy-modified trifunctional aliphatic urethane acrylate, one kind in six functional groups aliphatic urethane acrylate or several
Kind.Such as the carboxyl acid modified trifunctional aliphatic urethane acrylate of Shenzhen ComeOn brightness Chemical Industry Science Co., Ltd
UV4900；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；It
The carboxy-modified aliphatic urethane acrylate of the hydroxyl modification trifunctional of Tianjin glycolylurea Ci Co., Ltd 5652；The limited public affairs in Changxing
The difunctional hydroxyl modification two of department can roll into a ball aliphatic urethane acrylate DU-U153, six functional groups aliphatic polyurethane third
Olefin(e) acid ester 6146-100；Six functional groups group aliphatic polyurethane CN9010NS of Sartomer etc..Resin is glue performance
Major embodiment person not only coordinates the function of each component in glue system, makes to play collaboration facilitation between each component, avoid
A certain component brings the defect that overall performance declines, while itself mainly undertaking being bonded after film-forming, cold-resistant thermal shock, resistance to
The basic performances such as time, resistant to chemical etching.More important is the resin system of present invention compositions rationally, keeps glue System forming unified
Harmonious organic whole.Aliphatic urethane acrylate has that toughness is good, shrinking percentage is low, higher reactivity and functional group
The advantages that, the especially polarity connection of the aliphatic urethane acrylate after percarboxylic acids or hydroxyl modification and glass baseplate
Closely, can there are certain adhesive force, the also performance with chemical attacks such as ethanol-tolerants with glass baseplate；Meanwhile it introducing hydrophilic
Carboxyl, hydroxyl polar group are additionally favorable for by pure water neutrality developing liquid developing.It is attached to solve hardly possible of the glue on cover-plate glass base material
Problem, the problem resistant to chemical etching such as water boiling resistance and ethanol-tolerant is improved, washing developing liquid developing ability is improved, to take into account water
Property and solvent type develop two ways.
In the present invention, acrylated phosphate class compound is methacrylic acid phosphoric acid ester, 2- hydroxyethyl methacrylic acid phosphorus
One or more of acid esters, methylacryoyloxyethyl phosphate；It is preferred that 2- hydroxyethyl methacrylic acid phosphates；The present invention
High acid value acrylate analog assistant carry abundant polar group, reactivity is strong, in glue curing, acrylate analog assistant
Carbon-carbon double bond itself that contain participates in curing reaction, while the polar group of institute's band can be with the silica in the inorganic substrates such as glass
Key chemically reacts, and forms very big active force, is effectively increased the adhesive force of glue and glass baseplate, solves existing
There is glue that can not form the problem of strong active force with inorganic substrate.And polar group is also beneficial to pure water development, to simultaneous
Care for aqueous and solvent type development two ways.
In the present invention, esters of acrylic acid activated monomer is 2-Hydroxy ethyl acrylate, iso-bornyl acrylate, propylene
Acid -2- hydroxy propyl esters, ethoxyquin trimethylolpropane trimethacrylate, 1,6- hexanediyl esters, Isosorbide-5-Nitrae-hexylene glycol two
One or more of acrylate, 1,4-butanediol diacrylate, dipentaerythritol hexaacrylate.Activated monomer can be with
Regulation system viscosity so that each component is uniformly dispersed, and increases the interface synergistic effect between each component, to obtain comprehensive performance
Excellent glue.Simultaneously as the diluent with active group, such as its hydroxy functional group of 2-Hydroxy ethyl acrylate and tree
Fat main body the chemical bond with the inorganic substrates such as polar group and glass (such as its internal silicon oxygen bond) chemistry can be formed
Key active force significantly increases the adhesive force of transfer glue and base material.
In the present invention, photoinitiator be -2 methyl-1 phenyl -1- acetone of 2- hydroxyls, benzoin dimethylether, phenyl it is bis- (2,4,
6- trimethylbenzoyls) phosphine oxide, 2,4,6- trimethylbenzoy-dipheny phosphine oxides, 1- hydroxy-cyclohexyl-phenyls
One or more of ketone, benzophenone, 2- methyl-1s-[4- (methyl mercapto) phenyl] -2- morpholinyl -1- acetone.It is light-initiated
The LED light Spectral matching of 365nm wavelength is fixed in agent with cold light source, is utmostly played photoinitiation, can be fully absorbed light source,
Cross-linking reaction is generated free radicals, glue is fully cured, and ensures its performance.
In the present invention, silane coupling agent is vinyltrimethoxysilane, vinyltrimethoxysilane, triethoxy first
One or more of base silane, 3- methacrylic acids propyl three (trimethyl silane).Coupling agent dosage is smaller, but it is in glue
Can increase in aqueous systems with cover-plate glass substrate interface active force, as trying to make a match fill up high-molecular compound interchain
Gap effectively improves the water boiling resistance performance after transfer adhesive curing.
In the present invention, a length of 365nm of LED light wave.The LED light of fixed wave length, environmental-friendly, not heat release substantially, energy are non-
Often stablize, it is serious to solve existing curing mode heat release, and energy of light source fluctuation is larger, is unfavorable for asking for product volume production stability
Topic.
Preferably, by weight, cover-plate glass base material LED light cures no-solvent type sensitive transfer glue by following
Group is grouped as：
The invention also discloses the above-mentioned cover-plate glass base material preparation sides of LED light solidification no-solvent type sensitive transfer glue
Method includes the following steps：
(1) by aliphatic polyurethane acrylate, 80-90%, the photoinitiator of esters of acrylic acid activated monomer gross mass
It is sequentially added in container with acrylate phosphate class compound, mixing, dispersion, filtering obtain host agent；
(2) residual acrylic acid esters activity diluting monomer, silane coupling agent are sequentially added in container and is mixed, dispersion, mistake
Filter, obtains adjuvant；
(3) in mass ratio 10: 1 mixing host agents and adjuvant, dispersion, filtering cure to get to cover-plate glass base material LED light
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 hours；In step (2), dispersion
Rate is that 200-500 turns/min, and the time is 0.5-1 hours；In step (3), dispersion rate is that 200-500 turns/min, and the time is
0.5-1 hours；In step (1), step (2) and step (3), the environment of dispersion be protected from light, ventilated environment, temperature is
15-35℃。
Above-mentioned cover-plate glass base material cures no-solvent type sensitive transfer glue with LED light and can be applied to the transfer of cover-plate glass base material
Processing, includes the following steps：It is coated with cover-plate glass base material LED light in cover-plate glass substrate surface and cures no-solvent type sense
Light transfer glue；Then film diaphragm is covered again；Then LED light source 100-200mJ/cm is used2Low energy precuring exposes；Then
Film diaphragm is removed, the not photosensitive part glue of developing solution dissolution is used；Then dry up or dry residual developer solution；Finally use
LED light source 1000-2000mJ/cm2Transfer glue after the development of high-energy secondary curing, i.e., at the transfer of completion cover-plate glass base material
Reason；The developer solution is water or organic solvent type developer solution；Preferably water.
Wherein pure water developer solution is non-combustible, no organic matter volatilization, non-explosive；Organic solvent developer solution by ethyl alcohol, normal propyl alcohol,
One or more of isopropanol, n-butanol, isobutanol or n-amyl alcohol form.
Glue construct and film forming procedure in a series of physical, chemical change can occur, these variations and glue itself
Property adds the difference of construction parameter, may significantly affect the application performance of glue.For example, after glue application, it may appear that
New interface, if the interfacial tension at the liquid/solid interface between glue and material is higher than the critical surface tension of material, glue is just
It can not smoothly be sprawled on material, will produce the bad defect such as flake, shrinkage cavity；When solvent-laden adhesive curing, because of curing exotherm, meeting
Promote solvent volatilization, will can cause between film surface and inside generate temperature, density and surface tension it is poor, these are poor
It is different and then cause to generate the turbulent motion inside glued membrane, form so-called vortex, vortex can cause to generate the bad phenomenons such as tangerine peel；
In curing system, there is more than a kind of resins, it is possible to generate insoluble micelle in solidification process, lead to surface tension gradient
It is formed.Activity diluting monomer, resin oligomers, each analog assistant in special glue composition, all there may be carry to enrich reactive group
Group the case where, between macromolecule resin oligomer, small molecule active diluting monomer, auxiliary agent reactivity it is uncertain, glue prepare,
All there are a variety of reactions in solidification process, this situation can cause glue to be coated in material surface, after solidification, every physics of glue,
Chemical property is unstable.
The invention devises new glue system, resin and additive, particular with its of active group
Compatibility is good between remaining compound, and the component for generating adverse chemical reaction separately stores, and ensures the storage stability of glue.And
Glue not will produce side reaction in preparation and solidification substantially between organic matter, guarantee glue is anti-with cover-plate glass material surface
Activity is answered, improves the interface interaction power of glue and material, effectively increases the bonding force of glue/material.Glue system stability
It is good, it is unlikely to deteriorate, after storage, in the case of temperature-resistant, viscosity does not change substantially；Reactivity is good when solidification, double bond
Conversion ratio is high, and coating performance is good；After glue curing, the corrosive powers such as ethanol-tolerant are strong, and the weatherability having had, for a long time not
Discoloration is faded；It is not easy xanthochromia.Cured glue layer has excellent bonding force to material, solves glue in nothings such as cover-plate glass
On machine base material the problem of difficult attachment.
In addition, the prior art reduces drawbacks described above to the greatest extent, can be applied in glue to improve the interfacial effect of glue and base material
Base material is pre-processed before cloth；Thoroughly ensure the cleaning of base material.Glue is directly passed through newly-designed sensitive transfer process by the present invention
It constructs, the glue-line after solidification is good with substrate bonding, no boundary defect, ensure that the special lines requirement of product and appearance
Meanwhile the ability resistant to chemical etching such as water boiling resistance and ethanol-tolerant for effectively increasing base material.
Since above-mentioned technical proposal is used, the present invention has following advantages compared with prior art：
1. the present invention first public cover-plate glass base material LED light cures no-solvent type sensitive transfer glue, design is unique,
Composition is reasonable, and it is convenient to prepare, and is in turn ensured while improving glue cementability performance with base material adhesive force with excellent
The special lines appearance requirement of cover-plate glass, improves water boiling resistance, chemical resistance, while environmentally friendly.
2. cover-plate glass base material disclosed by the invention cures no-solvent type sensitive transfer glue with LED light only needs very thin glue
Layer, it is only necessary to 6-10 microns, still achieve excellent cementability and water boiling resistance, chemical resistance, boiling water boiling 10 minutes, glue-line
Surface is no different shape, and adhesive force is still more than 4B, overcome it is existing need thicker glue-line cannot still improve chemical resistance,
The defect of water boiling resistance achieves unexpected technique effect.
3. cover-plate glass base material provided by the invention LED light cures no-solvent type sensitive transfer glue and passes through fixed 365nm
The LED light of wavelength cures, environmental-friendly, not heat release substantially, energy stabilization, has abandoned environmentally harmful, and disadvantage is significantly high
Pressure mercury lamp, high-pressure halogen lamp.
4. cover-plate glass base material provided by the invention LED light cures no-solvent type sensitive transfer glue and is free of solvent, still
Each component compatibility is good, and harmony is good between organic matter, no aggregation phenomenon, avoids a certain component itself advantage and disadvantage band outstanding
The defect that the glued membrane overall performance come declines；Simultaneously under the effect of each reactive group synergistic effect, resin system solidification effect is good,
Certain heat-resisting, chemically-resistant are obtained, mechanical property improves, and special organic matter reacts with mineral surfaces, interface interaction
Power is high, to obtain the glued membrane of the excellent combination properties such as adhesive force, rub resistance, solvent resistant, weatherability.
5. fat is added in acrylate analog assistant, esters of acrylic acid activated monomer, silane coupling agent by the invention
It in fat adoption urethane acrylate, sequentially adds, each component supplements and complements each other, and maximizes favourable factors and minimizes unfavourable ones, and meeting reactive component separately stores；Simultaneously
Each component institute band polar group can increase respective intermolecular forces, but not overreaction, ensure organic-compound system with it is inorganic
The reactivity of base material, to which while improving glue with material adhesive force, the glued membrane after solidification still has excellent synthesis
Performance.
6. cover-plate glass base material provided by the invention is used with LED light solidification no-solvent type sensitive transfer glue and the side of storage
Just, it and under the premise of meeting high bonding requirements, only need to once be coated with, thickness is thin, and dosage is few, friendly to the pollution of environment,
It is lower to the injury of human body；And since resin composition is reasonable, glue curing reactivity is good, the glue-line comprehensive performance after solidification
It is good, pure water neutrality developer solution or solvent type developing liquid developing can be used, be more suitable for industrialized production.Especially pure water develops, this
Kind visualization way environmental sound is the mainstream of futurity industry metaplasia production.
Description of the drawings
Fig. 1 is the front and back photo figure of one product adhesive force of embodiment test；
Fig. 2 is the front and back outside drawing of two product of embodiment, 150 DEG C of bakings；
Fig. 3 is the front and back photo figure of the resistance to ethyl acetate test of three product of embodiment；
Fig. 4 is the front and back photo figure of example IV product high temperature and humidity test；
Fig. 5 is the front and back photo figure of five product thermal shock of embodiment test.
Specific implementation mode
The invention will be further described with reference to the accompanying drawings and embodiments：
Embodiment one
By weight, by the carboxy-modified aliphatic poly ammonia of the hydroxyl modification trifunctional of 40 parts of Tianjin glycolylurea Ci Co., Ltd
The carboxyl acid modified trifunctional aliphatic polyurethane third of 5652,10 parts of Shenzhen ComeOn brightness Chemical Industry Science Co., Ltd of ester acrylate
Olefin(e) acid ester UV4900,41 parts of iso-bornyl acrylate activated monomers, 1 part of phenyl bis- (2,4,6- trimethylbenzoyls) oxidation
Phosphine, 1 part 2,4,6- trimethylbenzoy-dipheny phosphine oxides, 2 parts of benzophenone, 5 parts of 2-hydroxyethyl methacrylate phosphorus
Acid esters auxiliary agent sequentially adds in stirring dispersion machine, normal pressure, 25 DEG C, be protected from light, dry, ventilated environment, in 1000 revs/min stir 4
Hour, it is dispersed with stirring uniformly, filters clean impurity, be protected from light, pack, be host agent；
By weight, by 3 parts of iso-bornyl acrylates, 2 parts of 1,6- hexanediyl esters, 2 parts of vinyl front threes
Oxysilane, 3 parts of 3- methacrylic acids propyl three (trimethyl silane) sequentially add in stirring dispersion machine, normal pressure, 25 DEG C, keep away
Light, drying, ventilated environment stir 0.5 hour in 500 revs/min, are dispersed with stirring uniformly, filter clean impurity, be protected from light, seal
Packaging is adjuvant；
Take above-mentioned host agent and adjuvant, mass ratio 10: 1 to sequentially add in stirring dispersion machine respectively, normal pressure, 35 DEG C, keep away
Light, drying, ventilated environment stir 1 hour in 400 revs/min, are dispersed with stirring uniformly, filter clean impurity to get to cover board glass
Glass base material cures no-solvent type sensitive transfer glue with LED light.
Embodiment two
By weight, by the carboxy-modified aliphatic poly ammonia of the hydroxyl modification trifunctional of 40 parts of Tianjin glycolylurea Ci Co., Ltd
5652,41 parts of iso-bornyl acrylates of ester acrylate, 10 parts of Sartomers six functional groups aliphatic polyurethane propylene
Sour fat CN9010NS, 2 part 2,4,6- trimethylbenzoy-dipheny phosphine oxides, 2 parts of benzophenone, 5 parts of 2- hydroxyethyl methyls
Acrylate phosphate auxiliary agent sequentially adds in stirring dispersion machine, normal pressure, 35 DEG C, be protected from light, dry, ventilated environment, in 1000 turns/
Minute stirring 4 hours, is dispersed with stirring uniformly, filters clean impurity, be protected from light, pack, and is host agent；
By weight, by 3 parts of 2-Hydroxy ethyl acrylates, 2 parts of 1,6- hexylene glycols and acrylate, 2 parts of vinyl front threes
Oxysilane, 3 parts of triethoxy methyl silicanes sequentially add in stirring dispersion machine, normal pressure, 25 DEG C, be protected from light, dry, venting ring
Border is stirred 0.5 hour in 500 revs/min, is dispersed with stirring uniformly, is filtered clean impurity, be protected from light, pack, and is adjuvant；
Take above-mentioned host agent and adjuvant, mass ratio 10: 1 to sequentially add in stirring dispersion machine respectively, normal pressure, 25 DEG C, keep away
Light, drying, ventilated environment stir 0.8 hour in 300 revs/min, are dispersed with stirring uniformly, filter clean impurity, i.e. cover-plate glass
Base material cures no-solvent type sensitive transfer glue with LED light.
Embodiment three
By weight, by the carboxy-modified aliphatic poly ammonia of the hydroxyl modification trifunctional of 45 parts of Tianjin glycolylurea Ci Co., Ltd
The six functional groups aliphatic urethane acrylate 6146-100,41 parts of different ice of 5652,5 parts of Changxing Co., Ltds of ester acrylate
Chip base acrylate reactive monomer, 2 part 2,4,6- trimethylbenzoy-dipheny phosphine oxides, 2 parts of 1- hydroxy-cyciohexyls-benzene
Base ketone, 5 parts of 2-hydroxyethyl methacrylate phosphate adjuvants sequentially add in stirring dispersion machine, normal pressure, 25 DEG C, be protected from light,
Dry, ventilated environment stirs 4 hours in 1000 revs/min, is dispersed with stirring uniformly, filters clean impurity, be protected from light, pack,
For host agent；
By weight, by 2 parts of vinyltrimethoxysilanes, 3 parts of triethoxy methyl silicanes, 5 parts of acrylic acid -2- hydroxyls
Propyl ester sequentially adds in stirring dispersion machine, normal pressure, 25 DEG C, be protected from light, dry, ventilated environment, in 500 revs/min stir 1 hour,
It is dispersed with stirring uniformly, filters clean impurity, be protected from light, pack, be adjuvant；
Take above-mentioned host agent and adjuvant, mass ratio 10: 1 to sequentially add in stirring dispersion machine respectively, normal pressure, 25 DEG C, keep away
Light, drying, ventilated environment stir 0.8 hour in 300 revs/min, are dispersed with stirring uniformly, filter clean impurity to get to cover board
Glass baseplate cures no-solvent type sensitive transfer glue with LED light.
Example IV
By weight, by the carboxy-modified aliphatic poly ammonia of the hydroxyl modification trifunctional of 30 parts of Tianjin glycolylurea Ci Co., Ltd
The hydroxyl modification two of 5652,15 parts of good photochemical Science and Technology Ltd.s of Shenzhen ancient cooking vessel of ester acrylate can roll into a ball aliphatic polyurethane acrylic acid
Ester DH-305,5 parts of Sartomers six functional groups aliphatic polyurethane acrylate CN9010NS, 35 parts of isobornyls
Acid esters activated monomer, 6 parts of 2-Hydroxy ethyl acrylates, 2 part 2,4,6- trimethylbenzoy-dipheny phosphine oxides, 2 parts of 1-
Hydroxy-cyclohexyl-phenyl ketone, 5 parts of 2-hydroxyethyl methacrylate phosphate adjuvants sequentially add in stirring dispersion machine, often
Pressure, 25 DEG C, be protected from light, dry, ventilated environment, in 1000 revs/min stir 4 hours, be dispersed with stirring uniformly, filter clean impurity,
It is protected from light, packs, be host agent；
By weight, by 2 parts of vinyltrimethoxysilanes, 3 parts of triethoxy methyl silicanes, ethoxyquin trihydroxy methyl third
Alkane triacrylate sequentially adds in stirring dispersion machine, normal pressure, 25 DEG C, be protected from light, dry, ventilated environment, stirred in 500 revs/min
It mixes 1 hour, is dispersed with stirring uniformly, filters clean impurity, be protected from light, pack, be adjuvant；
Take above-mentioned host agent and adjuvant, mass ratio 10: 1 to sequentially add in stirring dispersion machine respectively, normal pressure, 25 DEG C, keep away
Light, drying, ventilated environment stir 0.8 hour in 300 revs/min, are dispersed with stirring uniformly, filter clean impurity to get to cover board
Glass baseplate cures no-solvent type sensitive transfer glue with LED light.
Embodiment five
By weight, by the carboxy-modified aliphatic poly ammonia of the hydroxyl modification trifunctional of 35 parts of Tianjin glycolylurea Ci Co., Ltd
The difunctional hydroxyl modification two of 5652,10 parts of Changxing Co., Ltds of ester acrylate can roll into a ball aliphatic urethane acrylate
DU-U1535 parts, six functional groups aliphatic polyurethane acrylate CN9010NS, the 36 parts of isobornyls third of 5 parts of Sartomers
Olefin(e) acid ester activated monomer, 5 parts of ethoxyquin trimethylolpropane trimethacrylates, 2 part 2,4,6- trimethylbenzoy-diphenies
Phosphine oxide, 2 parts of 1- hydroxy-cyclohexyl-phenyls ketones, 5 parts of 2-hydroxyethyl methacrylate phosphate adjuvants are sequentially added and are stirred
Mix in dispersion machine, normal pressure, 25 DEG C, be protected from light, dry, ventilated environment, in 1000 revs/min stir 4 hours, be dispersed with stirring uniformly,
Clean impurity is filtered, is protected from light, packs, is host agent；
By weight, by 2 parts of vinyltrimethoxysilanes, 3 parts of 3- methacrylic acids propyl three (trimethyl silane), second
Oxidation trimethylolpropane trimethacrylate, 3 parts of 2-Hydroxy ethyl acrylates sequentially add in stirring dispersion machine, normal pressure, 25
DEG C, be protected from light, dry, ventilated environment, in 500 revs/min stir 1 hour, be dispersed with stirring uniformly, filter clean impurity, be protected from light, be close
Package fills, and is adjuvant；
Take above-mentioned host agent and adjuvant, mass ratio 10: 1 to sequentially add in stirring dispersion machine respectively, normal pressure, 25 DEG C, keep away
Light, drying, ventilated environment stir 0.8 hour in 300 revs/min, are dispersed with stirring uniformly, filter clean impurity to get to cover board
Glass baseplate cures no-solvent type sensitive transfer glue with LED light.
Above-mentioned cover-plate glass base material is cured into no-solvent type sensitive transfer glue with LED light and carries out following technique to glass baseplate
Transfer process：
1, embodiment one to four uses pure water neutrality developing liquid developing mode technique：
Glue is coated on cover-plate glass material surface；The film diaphragm containing grain pattern is covered, film diaphragm has and can expose
Light region and black occlusion area；Film diaphragm, glue, material are closely pressed by rubber roller；Use fixed 365nm wavelength
LED light carries out precuring exposure, precuring energy：100-200mJ/cm2；Film diaphragm is thrown off, is then developed by pure water；It dries
Dry film surface developer solution, baking condition：85-95 DEG C of baking 15min；Secondary curing, profound solidification energy：1000-
2000mJ/cm2, the performance tests such as physics, chemistry are carried out to glue-line.
2, embodiment five uses solvent type developing liquid developing mode technique：
Glue is coated on cover-plate glass material surface；The film diaphragm containing special grains pattern is covered, film diaphragm has
It can exposure area and black occlusion area；Film diaphragm, glue, material are closely pressed by rubber roller；Use 365nm wavelength
LED light carries out precuring exposure, precuring energy：180mJ/cm2；Throw off film diaphragm, then by by isometric ethyl alcohol, just
The solvent type developing liquid developing of propyl alcohol, isopropanol, n-butanol, isobutanol, n-amyl alcohol composition；It is aobvious using spray gun drying film surface
Shadow liquid, process conditions：28 DEG C, the spray gun of 1.1MPA pressure blows 8min；Secondary curing, profound solidification energy：1800mJ/cm2,
The performance tests such as physics, chemistry are carried out to glue-line.
No-solvent type sensitive transfer glue is cured with LED light to above-mentioned cover-plate glass base material and carries out following items test：Film thickness,
Film thickness gauge；Appearance, range estimation and 60 times of magnifying glasses；Hardness, cart type pencil hardometer, load 750g；Ethanol-tolerant, embodiment glue
Room temperature is after 24 hours after solidification, by glue be placed in ventilation, cool place, 25 DEG C of environment alcoholic solution in impregnate 10min；Resistance to second
Room temperature is after 24 hours after acetoacetic ester, glue curing, by glue be placed in ventilation, cool place, 25 DEG C of environment ethyl acetate solution
Middle immersion 10min；Room temperature is after 24 hours after high-temp resisting high-humidity resisting, glue curing, is placed in 85 DEG C of temperature, under 85% environment of humidity
It places 72 hours；Adhesive force test is drawn using film surface of the sharp cutter (15~30 ° of knife edge angle) after embodiment solidification
The square small grid of 10 × 10 1mm × 1mm, every scribing line depth and glue-line bottom, touch glass surface.It will using banister brush
The fragment of test zone is clean, then firmly clings net using 3M companies No. 600 adhesive tapes (300~400g/cm2 of adhesion strength)
Lattice region 30 seconds, holds adhesive tape one end, and adhesive tape is shut down rapidly in vertical direction (90 °).Same position, same method test
3 times；Room temperature first places -16 DEG C of environment and keeps 30min, then quickly rise after 24 hours after cold-resistant thermal shock, glue curing
It is 1 cycle that temperature keeps 30min to 80 DEG C, totally 10 cycles；Room temperature 24 hours after water boiling resistance, embodiment glue curing
Afterwards, 100 DEG C of thermostat water bath 10min are put into, is then allowed to stand and dries 0.5 hour, ensure glue-line drying；Low temperature resistant, embodiment glue
- 16 DEG C of environment are positioned over after water cure；150 DEG C of baking 30min are carried out after high temperature resistant, embodiment glue curing；It is water-fast after high temperature
It boils after carrying out 150 DEG C of baking 30min after performance, embodiment glue curing, is put into 100 DEG C of thermostat water bath 30min, then uses
Non-dust cloth wipes surface, dries and stands 3-5min.
Above-mentioned cover-plate glass base material LED light cures test result such as table 1 after no-solvent type sensitive transfer adhesive curing.
1 test result of table
Attached drawing 1 is the front and back photo figure of one product adhesive force of embodiment test, it can be seen that provides attachment according to the present invention
Power testing standard is determined as 5B.
Attached drawing 2 is the front and back outside drawing of two product of embodiment, 150 DEG C of bakings, it can be seen that the front and back appearance of baking is not existing apparent
Variation.
Attached drawing 3 is the front and back photo figure of the resistance to ethyl acetate test of three product of embodiment, it can be clearly seen that, according to the present invention
The resistance to ethyl acetate test of transfer glue prepared by method does not show abnormal appearance.
Attached drawing 4 is the front and back photo figure of example IV product high temperature and humidity test, it can be clearly seen that, according to present invention side
After transfer glue high temperature and humidity test prepared by method, not existing abnormal appearance.
Attached drawing 5 is the front and back photo figure of five product thermal shock of embodiment test, it can be clearly seen that, according to present invention side
After transfer glue thermal shock prepared by method, not existing abnormal appearance.
According to above-mentioned transfer glue treated cover-plate glass base material figure, it can be seen that：Because cover-plate glass can not be cut, therefore
Product of the present invention solves the problems, such as cover-plate glass excessive glue, meanwhile, the front camera hole on such as front glass top does not need glue
Water covers, and product of the present invention also smoothly solves the problems, such as this；And each hole on cover-plate glass is very round, and is covered without glue
Lid.
Claims (7)
1. a kind of cover-plate glass base material cures no-solvent type sensitive transfer glue with LED light, it is characterised in that：By weight, institute
It is composed of the following components to state cover-plate glass base material LED light solidification no-solvent type sensitive transfer glue：
The aliphatic urethane acrylate is hydroxyl modification difunctional fat adoption urethane acrylate, carboxy-modified three
It is several in functional group's aliphatic urethane acrylate, six functional groups aliphatic urethane acrylate；And the aliphatic
Urethane acrylate contains hydroxyl modification difunctional fat adoption urethane acrylate and/or carboxy-modified trifunctional fat
Fat adoption urethane acrylate；
The silane coupling agent is vinyltrimethoxysilane and triethoxy methyl silicane.
2. cover-plate glass base material cures no-solvent type sensitive transfer glue with LED light according to claim 1, it is characterised in that：
The acrylated phosphate class compound is methacrylic acid phosphoric acid ester, 2- hydroxyethyl methacrylic acids phosphate, metering system
One or more of acyloxyethyl phosphate.
3. cover-plate glass base material cures no-solvent type sensitive transfer glue with LED light according to claim 1, it is characterised in that：
The esters of acrylic acid activated monomer be 2-Hydroxy ethyl acrylate, iso-bornyl acrylate, 2-hydroxypropyl acrylate,
Ethoxyquin trimethylolpropane trimethacrylate, 1,6- hexanediyl esters, Isosorbide-5-Nitrae-hexanediyl ester, Isosorbide-5-Nitrae-fourth
One or more of omega-diol diacrylate, dipentaerythritol hexaacrylate.
4. cover-plate glass base material cures no-solvent type sensitive transfer glue with LED light according to claim 1, it is characterised in that：
The photoinitiator is -2 methyl-1 phenyl -1- acetone of 2- hydroxyls, benzoin dimethylether, bis- (2,4, the 6- trimethylbenzene first of phenyl
Acyl group) phosphine oxide, 2,4,6- trimethylbenzoy-dipheny phosphine oxides, 1- hydroxy-cyclohexyl-phenyls ketone, hexichol first
One or more of ketone, 2- methyl-1s-[4- (methyl mercapto) phenyl] -2- morpholinyl -1- acetone.
5. cover-plate glass base material cures no-solvent type sensitive transfer glue with LED light according to claim 1, which is characterized in that
By weight, it is composed of the following components to cure no-solvent type sensitive transfer glue for cover-plate glass base material LED light：
6. any one cover-plate glass base material described in claim 1-5 cures the preparation of no-solvent type sensitive transfer glue with LED light
Method, which is characterized in that include the following steps：
(1) by aliphatic urethane acrylate, the 80-90% of esters of acrylic acid activated monomer gross mass, photoinitiator and third
Olefin(e) acid ester phosphate compounds sequentially add in container, and mixing, dispersion, filtering obtain host agent；
(2) residual acrylic acid esters activity diluting monomer, silane coupling agent are sequentially added in container and is mixed, disperseed, filter, obtain
To adjuvant；
(3) in mass ratio 10: 1 mixing host agents and adjuvant, dispersion, filtering cure to get to cover-plate glass base material LED light without molten
Dosage form sensitive transfer glue；
In step (1), dispersion rate is that 1000-1500 turns/min, and the time is 1-4 hours；In step (2), dispersion rate is
200-500 turns/min, and the time is 0.5-1 hours；In step (3), dispersion rate is that 200-500 turns/min, and the time is that 0.5-1 is small
When；In step (1), step (2) and step (3), the environment of dispersion be protected from light, ventilated environment, temperature is 15-35 DEG C.
7. the LED light of any one cover-plate glass base material described in claim 1-5 cures no-solvent type sensitive transfer glue in cover board
Application in glass baseplate transfer process, it is characterised in that：Developer solution is water when the transfer process.
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| CN105331324B (en) * | 2015-11-20 | 2018-02-13 | 烟台信友新材料股份有限公司 | A kind of free radical type ultraviolet cured adhesive and preparation method for optical alignment |
| CN105820794A (en) * | 2016-05-30 | 2016-08-03 | 三友（天津）高分子技术有限公司 | Inorganic filler modified ultraviolet curing adhesive |
| CN106867373A (en) * | 2017-03-28 | 2017-06-20 | 惠州市潮新科数字器材科技有限公司 | The photosensitive glue compositions of UV and its application in exempting from electrochemical treatments CTP editions |
| CN106928896A (en) * | 2017-03-28 | 2017-07-07 | 南雄市毅豪化工有限公司 | A kind of acidproof edge sealing adhesive of ultraviolet light polymerization |
| PL235723B1 (en) * | 2017-08-07 | 2020-10-05 | Univ West Pomeranian Szczecin Tech | Method for producing adhesive bond and the structural, photocuring adhesive for glass |
| PL235722B1 (en) * | 2017-08-07 | 2020-10-05 | Zachodniopomorski Univ Technologiczny W Szczecinie | Method for producing adhesive bond and the structural, photocuring UV adhesive for glass |
| CN107936905B (en) * | 2017-11-28 | 2018-08-28 | 黑龙江天有为电子有限责任公司 | Segment encode liquid crystal display and TFT liquid crystal screen combined instrument cover board joint adhesive and applying method |
| CN108517196A (en) * | 2018-04-16 | 2018-09-11 | 苏州市贝特利高分子材料股份有限公司 | Sapphire glass base material with can photosensitive development special grains transfer glue and preparation method thereof |
| CN109266281A (en) * | 2018-08-15 | 2019-01-25 | 瑞声科技(新加坡)有限公司 | UV glue |
| CN110964476B (en) * | 2018-09-30 | 2022-01-04 | 惠州比亚迪实业有限公司 | Ultraviolet light curing adhesive composition, transfer curing adhesive and preparation method |
| CN109203752A (en) * | 2018-10-17 | 2019-01-15 | 刘剑 | A kind of GDM technique |
| CN110343504A (en) * | 2019-06-28 | 2019-10-18 | 深圳日高胶带新材料有限公司 | A kind of light-cured type pressure sensitive adhesive of resistance to ultralow temperature |
| CN110582176B (en) * | 2019-10-12 | 2021-05-07 | Oppo广东移动通信有限公司 | Shell, manufacturing method thereof and electronic equipment |
| CN111916249B (en) * | 2020-06-30 | 2022-05-20 | 嘉兴中科枫林生物技术有限公司 | High-performance flexible electronic functional base material |
| CN113549179B (en) * | 2021-07-22 | 2023-11-17 | 连云港华海诚科电子材料有限公司 | Red high thixotropic UV adhesive for manufacturing gasket and preparation method thereof |
| CN115717043A (en) * | 2022-11-02 | 2023-02-28 | 佛山阳光逸采涂料科技有限公司 | Ultraviolet light curing adhesive and preparation method and application thereof |
| CN116904127B (en) * | 2023-07-04 | 2024-06-04 | 江苏特丽亮新材料科技有限公司 | Double-sided high-temperature-resistant UV (ultraviolet) mucous membrane reducing and preparation method thereof |
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| DE102012023181A1 (en) * | 2012-11-28 | 2014-05-28 | Basf Se | Producing two-layer foam plates used for manufacturing rotor blades of wind turbines, comprises bonding two thinner foam sheets to a two-layer foam sheet, where adhesive is applied on one of surfaces of the thinner foam sheets |
| CN104531043A (en) * | 2014-12-23 | 2015-04-22 | 广州市尤特新材料有限公司 | LED-UV curable reinforcing adhesive |
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