CN104151925B - High temperature resistant ink and preparation method thereof and OGS contact panels - Google Patents
High temperature resistant ink and preparation method thereof and OGS contact panels Download PDFInfo
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- CN104151925B CN104151925B CN201410351240.6A CN201410351240A CN104151925B CN 104151925 B CN104151925 B CN 104151925B CN 201410351240 A CN201410351240 A CN 201410351240A CN 104151925 B CN104151925 B CN 104151925B
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Abstract
The invention provides a kind of high temperature resistant ink, including：0.1～4 part of 100 parts of organic-silicon-modified resin, 60～240 parts of titanium dioxide, 0.5～10 part of aerosil, 1～30 part of cross-linking agent, 0.01～1 part of silanol condensation catalyst, 0.1～4 part of polysiloxane defoamer, alkyl and/or aralkyl modified polysiloxane levelling agent, 50～150 parts of solvent.In the oil resistant graphite product of the present invention, using organic-silicon-modified resin as major ingredient, coordinate with function additives such as specific cross-linking agent, silanol condensation catalyst, defoamer and levelling agents, the common heat-resisting quantity for lifting ink product, anti-yellowing, stability and other effects, obtain the excellent white glass ink product of high temperature resistant and chemical resistance.
Description
Technical field
The invention belongs to contact panel printing-ink technical field, and in particular to a kind of high temperature resistant ink and its preparation method
And OGS contact panels.
Background technology
In existing OGS (One Glass Solution, integral type touch-control) contact panel processing procedure, needed in ITO bases at first
On material print high temperature resistant ink, the hardness and chemical resistance on surface are controlled, realize rear operation effectively to conductive silver paste,
ITO coating, printing lithographic glue, exposure, development, etching ito film, stripping photoresist etc. are protected；And then can control attached
Put forth effort, hardness and demoulding time, can significantly lift yields.In above-mentioned processing procedure, resistant to elevated temperatures ink sheet is printed at first
Body can be processed through follow-up hot environment, developer solution, ITO etching solutions etc..Existing high temperature resistant ink major ingredient is at most used
With high-low temperature resistant, weather-resistant, high insulation resistance modifying epoxy resin by organosilicon；But these ink products are due to which
The molecular structure of major ingredient itself, easily turns yellow in the process of 250～300 DEG C of scope high temperature, for the display of OGS contact panels
Effect causes to have a strong impact on；And function additive is selected for major ingredient, is considered for stability in the large, viscosity, hardness etc., not
Ink can be made to have preferable effect and function at resistance to gentle anti-yellowing aspect.
The content of the invention
The above-mentioned deficiency for aiming to overcome that prior art of the embodiment of the present invention, there is provided a kind of resistance to elevated temperatures is more excellent,
The high temperature resistant ink not turned yellow in the range of 250～300 DEG C.
In order to realize foregoing invention purpose, the technical scheme of the embodiment of the present invention is as follows：
A kind of high temperature resistant ink, including each component of following mass parts：
100 parts of organic-silicon-modified resin, 60～240 parts of titanium dioxide, 0.5～10 part of aerosil, cross-linking agent 1～30
Part, 0.01～1 part of silanol condensation catalyst, 0.1～4 part of polysiloxane defoamer, alkyl and/or aralkyl modified poly-
0.1～4 part of organosiloxane levelling agent, 50～150 parts of solvent.
In the oil resistant graphite product of the present invention, using organic-silicon-modified resin as major ingredient, coordinate with specific cross-linking agent,
The function additives such as silanol condensation catalyst, defoamer and levelling agent, it is the common heat-resisting quantity for lifting ink product, anti-yellowing, steady
It is qualitative and other effects, obtain the excellent white glass ink product of high temperature resistant and chemical resistance.
The present invention further also proposes the preparation method of above-mentioned high temperature resistant ink, comprises the steps：
By 30～100 parts in the silicone modified polyester resin of 100 weight portion of raw material and Rutile type titanium dioxide, gas phase
After silicon dioxide is mixed with partial solvent, dispersed formation dispersed paste；
The dispersed paste is ground and is dispersed to fineness and is reached after less than 10 μm, added remaining organic-silicon-modified poly-
Ester resin, polysiloxane defoamer, alkyl and/or aralkyl modified polysiloxane levelling agent and partial solvent,
Uniformly mix to obtain ink host；
By cross-linking agent, silanol condensation catalyst and residual solvent mix homogeneously, ink solidification agent is obtained.
The present invention further also proposes the OGS contact panels prepared using above-mentioned high temperature resistant ink.
Using the above-mentioned high temperature resistant ink of the present invention, prepared by ink host and firming agent distribution, finally mixed again
Solidification, process are simple, and can substantially ensure that stable in properties, the effect of ink reach most preferably.And using the resistance to height of invention
OGS contact panels prepared by warm ink, after the techniques such as follow-up high temperature, plated film, etching, ink property does not change,
Nor can turn yellow；Display effect is more preferable.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein is not used to only to explain the present invention
Limit the present invention.
The embodiment of the present invention provides a kind of high temperature resistant ink, including each component of following mass parts：
100 parts of organic-silicon-modified resin, 60～240 parts of titanium dioxide, 0.5～10 part of aerosil, cross-linking agent 1～30
Part, 0.01～1 part of silanol condensation catalyst, 0.1～4 part of polysiloxane defoamer, alkyl and/or aralkyl modified poly-
0.1～4 part of organosiloxane levelling agent, 50～150 parts of solvent.
In the oil resistant graphite product of the present invention, using organic-silicon-modified resin as major ingredient, coordinate specifically to be crosslinked
The function additives such as agent, silanol condensation catalyst, defoamer and levelling agent, the common heat-resisting quantity for lifting ink product, it is anti-yellowing,
Stability and other effects, obtains the excellent white glass ink product of high temperature resistant and chemical resistance.
Wherein, contain at least one reactive silicon group in above-mentioned organic-silicon-modified molecular resin, the reactive silicon can be passed through
Group forms siliconoxygen bond and is cross-linked with each other.Reactive silicon group has the group that below general formula is represented：
In formula, R1And R2Represented from the alkyl that carbon number is 1～20, the aryl that carbon number is 6～20 independently of one another
Or the aralkyl that carbon number is 7～20.When reactive silicon group has multiple R1Or R2When, multiple R1Between or it is multiple
R2Between can be with identical, it is also possible to it is different.X represents hydroxyl or hydrolization group.When the reactive silicon group have it is multiple
X when, can be with identical between multiple X, it is also possible to different.In addition, m represents 1～3 integer, n represents 1～2 integer.
Wherein, when X is hydrolization group, can be from hydrogen atom, halogen atom, alkoxyl, acyloxy, ketoxime base etc.；
Wherein, from from the viewpoint of the mildness for keeping hydrolysis, preferred alkoxyl.
The above-mentioned Si modification resin of the present invention, in order to meet the effect for improving paint film crosslink density after solidification, in molecule preferably
Reactive silicon group containing 2 or more than 2.
The present invention ink in the organic-silicon-modified resin of major ingredient be with Si-O-Si keys as main chain, side chain carry organic group
Hybrid inorganic-organic macromolecular material.Si-O keys have very high bond energy (443.7kJ/mol), than common organic resin
In C-C keys bond energy (347.4kJ/mol) it is high, heat stability is good.In Si-O keys, the relative electronegativies of Si atoms and O atom are poor
It is different big, therefore Si-O keys polarity is big, has very high ionization tendency (51%), the alkyl to connecting on Si atoms has dipole to sense
Affect, improve stability of the connected alkyl of Si to Oxidation, that is to say, that oxidation of the Si-O-Si keys to these alkyl rises
To certain shielding action.Si-C keys bond energy is lower than C-C key bond energys, but d π-p π fit keys can be formed in Si-C, makes system
Energy is reduced, and the thermo oxidative stability of resin is improved.The C-C keys of common organic resin are low-molecular material by thermal oxide easy fracture,
And after the alkyl connected on Si atoms receives thermal oxide, generation is highly cross-linked more stable Si-O-Si keys, can prevent which
Main chain break degraded.All of these factors taken together causes organic-silicon-modified resin to have excellent thermo oxidative stability, in 250 DEG C of bars
After heating 24 hours under part, it is only 2%～8% that organic-silicon-modified resin is weightless.Organic-silicon-modified resin also has the resistance to of protrusion
Hou Xing, even if the also resistance to yellowing under ultraviolet acute irradiation.The major ingredient silicone modified polyester resin that the present invention is adopted is by anti-
, between different reactive silicon groups or with containing between active Si cross-linking agent, there is condensation reaction and take off in answering property silicon group
The small molecules such as eliminating water, alcohol, carboxylic acid, ketone, ketoxime, and form Si-O-Si keys.The result of Si-O-Si keys is formed, ink composite is made
With excellent resistance to elevated temperatures.
The silicone modified polyester resin adopted in the present invention, is at the end of polysiloxane main chain by polycondensation reaction
End or the upper polyester resin of side chain connection, form the copolymer of block, grafting or inierpeneirating network structure.With polyester resin adhesive force
The good advantage of good, chemical-resistant, the characteristics of there is organic siliconresin heatproof oxidation performance and excellent weatherability again, can with compared with
At low temperature, (200 DEG C of ＜) implements solidification.
In the oil resistant graphite product of the present invention, according to performance test and the requirement of using effect, machine silicon modified polyesterses
Resin accounts for the part by weight of high temperature resistant ink and controls 20～40%；If the content of silicone modified polyester resin is less than 20 weights
Amount part, the paint film mechanical strength formed after ink composite solidification are deteriorated.If the content of silicone modified polyester resin is higher than
40 weight portions, need to compress titanium dioxide in ink composite, cause content relatively low, the covering of the paint film formed after final solidification
Power is reduced.Based on said circumstances, the part by weight for most preferably controlling to account for high temperature resistant ink is 25～35%, can make various performances
Tend to balance stable, further ensure the overall performance of ink product.
Further, in the above-described embodiment, the titanium dioxide for adopting in the present invention is for Rutile type titanium dioxide, and controls
Particle diameter is in 0.15～0.50 μ m；The titanium dioxide of this type except itself can as brightening agent lifted color effects it
Outward, in itself particle diameter and type, with stable lattice, there are stronger reinforcement, anti-aging, filling effect after the addition, carry
Rise covering power.And titanium dioxide belongs to hydrophilic material, but its hygroscopicity is less strong, is more favorable for the superficiality of ink product.
Silicone modified polyester resin on consumption based on 100 weight portions, the consumption of Rutile type titanium dioxide is 60～240 weight portions
Select；Optimum Rutile type titanium dioxide be 100～200 weight portions, make ink entirety paint film mechanical performance and covering power it is comprehensive
The balance for closing performance reaches most preferably.
Aerosil in the further present invention, after adding aerosil on the basis of above-mentioned major ingredient, its
The special chemical inertness for possessing and special thixotropic property can be cooperateed with beneficial to ink bonding, rheological characteristic and thixotropy control；
Because the high temperature resistant ink of the present invention has the processes such as high temperature, etching in the follow-up processing procedure of OGS contact panels, in environmental change
In the case of difference is very big, prevents its performance from undergoing mutation necessary with regard to comparison, and the addition of aerosil can be realized
In the case of condition great change, it is ensured that ink delays suitable ability at aspects such as mobility.In the present invention, aerosil is
At least one in hydrophilic aerosil or hydrophobic type gas phase silica.And it is directed to the balance and stability of its property
Property, under the amount ratio of the silicone modified polyester resin based on 100 weight portions, the consumption of aerosil is 0.5～10 weight
Amount part；Optimum is 1～5 weight portion.
The cross-linking agent adopted in the present invention is selected from silane crosslinker, epoxy silane coupling, amino resins, polysilazane
In at least one.
Wherein, above-mentioned silane crosslinker of the invention is using with following structural formula：RnSiX4-n(n is 0～2 integer).
R is represented from the alkyl that carbon number is 1～10, the aryl that carbon number is 6～10 or aralkyl that carbon number is 7～10；
Such as methyl, ethyl, propyl group, isopropyl, butyl, isobutyl group, octyl group, phenyl, p-methylphenyl, benzyl etc..Work as crosslinked with silicane
When agent has two R groups in the molecule, R group can be with identical, it is also possible to different.X represent be selected from alkoxyl, acyloxy,
At least one in ketoxime base and alkenyloxy group.From the viewpoint of being easy to get from raw material, X is preferably methoxyl group, ethyoxyl, acetyl oxygen
At least one in base, butanone oximido, isopropyl alkenyloxy group.
The major ingredient adopted in the above-mentioned silane crosslinker that the present invention is adopted, with ink cooperates, in ink composite
When silane crosslinker meets steam, its alkoxyl, acyloxy, ketoxime base or alkenyloxy group can occur hydrolysis, form silanol base, can be with
There is condensation reaction with the reactive silicon group on silicone modified polyester resin, so as to form the Si-O-Si of excellent heat resistance
Key network；Finally interact to form cross-linked structure with the major ingredient of organosilicon modified polyester, improve the thermostability of paint film.On possessing
The silane crosslinker of structure is stated, MTMS, MTES, propyl trimethoxy silicon can be selected
It is alkane, propyl-triethoxysilicane, trimethoxysilane, isobutyl triethoxy silane, octyl group trimethoxy silane, pungent
Ethyl triethoxy silicane alkane, phenyltrimethoxysila,e, phenyl triethoxysilane, methyl silicate, tetraethyl orthosilicate, positive silicic acid
N-propyl, methyl triacetoxysilane, ethyltriacetoxysilane, propyl group triacetoxysilane, phenyl triacetyl oxygen
Base silane, dimethyl 2 acetoxyl group silane, four acetoxylsilanes, methyl tributanoximo silane, two diacetylmonoxime of dimethyl
Base silane, four butanone oximino silanes, phenyl tributanoximo silane, methyl three (isopropyl alkenyloxy group) silane, two (isopropyl of dimethyl
Alkenyloxy group) silane, four (isopropyl alkenyloxy group) silane, phenyl three (isopropyl alkenyloxy group) silane etc..
Wherein, above-mentioned epoxy silane coupling of the invention, can be selected from γ-(2,3- glycidoxy) propyl group front three
TMOS, γ-(2,3- glycidoxies) propyl-triethoxysilicane, γ-(2,3- glycidoxies) hydroxypropyl methyl diformazan
The mixture of one or more in TMOS, γ-(2,3- glycidoxies) hydroxypropyl methyl diethoxy silane.This class
Combination of the epoxy silane coupling of type with silane crosslinker with major ingredient is differed, but is also capable of achieving similar effect.
The alkoxyl of epoxy silane coupling can also be reacted with the reactive silicon group of silicone modified polyester resin, formed heat-resisting
The excellent Si-O-Si keys of property；The epoxy radicals of epoxy silane coupling are difficult to participate in reacting and open loop below 200 DEG C, work as temperature
When degree is more than 200 DEG C, epoxy radicals can be reacted with the silanol base on the reactive silicon group of silicone modified polyester resin, formed
The good Si-O-C keys of thermostability.
Wherein, the preferred highly methyl etherified amino resin of above-mentioned amino resins of present invention employing, height butyl etherificate ammonia
The mixture of one or more in the mixed etherified amino resins of base resin, highly etherification benzene substituted amino resins and height etherificate.
The mixed etherificate ammonia of this several amino resins camber methyl etherified amino resin, height butyl etherified amino resins and height etherificate
Base resin has following general structure：
Highly etherification benzene substituted amino resins have below general formula：
R in structure above represents methyl, normal-butyl or isobutyl
Base, multiple R can be with identical, it is also possible to different；R3Represent H atom or CH2OH groups (methylol).In these amino resins
Alkoxyl (OR groups) and methylol (CH2OH groups) contracting can occur with the reactive silicon group of silicone modified polyester resin
Reaction is closed, heat-resisting good Si-O-C keys are formed.
In the present invention, in cross-linking agent, a kind of last polysilazane has following structure：In formula
R is H atom or alkyl, and multiple R can be with identical, it is also possible to different.The polysilazane of this structural formula can be changed with organosilicon
Property polyester resin reactive silicon group on hydroxyl or by the hydrolization group hydrolysis on reactive silicon group the hydroxyl that formed
Base reacts, and forms the Si-O-Si keys of excellent heat resistance, and the imino group in polysilazane molecule and is discharged with the ammonia of small molecule
Go out.Reaction principle can be represented with following chemical equation：
Also there is a kind of high imino group resin in amino resins, with following structure：
R in formula represents methyl, normal-butyl or isobutyl group, many
Individual R can be with identical, it is also possible to different；The alkoxyl of high imino group resin can also be with the reaction of silicone modified polyester resin
Property silicon group there is condensation reaction, form the good Si-O-C keys of thermostability.But, containing more in high imino group molecular resin
Active imino group (- NH), be easily heated or ultraviolet irradiation affect, finally produce the defect of flavescence.Therefore, go out in use
In considering for contact panel function, high imino group resin is not adopted as far as possible, and above-mentioned imino group (- NH) is being carried out modifying replacement etc.
After processing, or after having corresponding solution avoid the problems referred to above, can be considered according to needed for effect.
The silanol condensation catalyst that the present invention is used can promote the hydroxyl of silicon atom bonding and the alcoxyl of silicon atom bonding
Condensation reaction between base, acyloxy, ketoxime base or alkenyloxy group, the finally effect in composition are interacted to combine with major ingredient and are carried
Rise the property of ink product.The silanol condensation catalyst used as the present invention selected from mineral acid, inorganic base, organic acid, have
At least one in machine amines, organo-metallic compound.
Wherein mineral acid, such as hydrochloric acid, sulphuric acid, nitric acid etc.；Inorganic base, such as sodium hydroxide, potassium hydroxide and ammonia etc.；
Organic acid, refers mainly to the organic carboxyl acid that carbon atom is 1～20, such as oxalic acid, formic acid, acetic acid, propanoic acid, octanoic acid, capric acid, benzoic acid
Deng；Organic amine compound, such as ethamine, ethylenediamine, n-hexylamine, triethylamine, triethanolamine, pyridine, 1,1,3,3- tetramethyl guanidine
Base propyl-triethoxysilicane, 1,1,3,3- tetramethyl guanidine radicals propyl trimethoxy silicanes, Tetramethylammonium hydroxide, tetraethyl hydrogen
Amine-oxides etc..
Organo-metallic compound, considers from the functional requirement for reducing dyeing, preferred organic group tin compound, organic group titanizing
Compound, organic group zirconium compoundss, organic group zinc compound and organic group aluminium compound, such as organic group tin compound, two Laurels
Sour dibutyl tin, dibutyltin diacetate, two sad dibutyl tins, dibutyitin maleate, dimethyl maleic acid dibutyl tin,
Dioctyl tin diacetate, distearyl acid dioctyl tin, tin dilaurate dioctyl tin, stannous octoate, dibutyltin oxide, oxidation two
Tin octylate, di-n-butyl double (acetylacetone,2,4-pentanedione) stannum, acetylacetone,2,4-pentanedione stannum；Organic group titanium compound, such as tetraisopropyl titanate, metatitanic acid
Four butyl esters, four (acetylacetone,2,4-pentanedione) titanium, diisopropoxy two (oacetic acid) titanium, two (acetoacetic acid) titanium of diisopropoxy and
Diisopropoxy bis(acetylacetonate) titanium etc.；Organic group zirconium compoundss, such as three n-butoxies (oacetic acid) zirconium, two just
Butoxy two (oacetic acid) zirconium, n-butoxy three (oacetic acid) zirconium, four (n-pro-pyl acetoacetic acid) zirconium, four
(acetoaceto acetic acid) zirconium, four (oacetic acid) zirconium, three n-butoxies (acetylacetone,2,4-pentanedione) zirconium, four (acetylacetone,2,4-pentanedione) zirconium；
Organic group zinc compound, such as zinc octoate, Zinc dibenzoate., p- p t butylbenzoic acid zinc, zinc naphthenate, Dodecanoic acid, zinc salt, Hard Fat
Sour zinc, zinc acetylacetonate etc.；It is organic group aluminium compound, such as aluminium methoxide, aluminium ethoxide, three isobutoxy aluminum, three different
Propoxyl group aluminum, diisopropoxy (oacetic acid) aluminum, two isobutoxies (oacetic acid) aluminum, diisopropoxy (second
Ethyl acetoacetic acid) aluminum, isopropoxy two (oacetic acid) aluminum, isopropoxy two (acetylacetone,2,4-pentanedione) aluminum, three (oacetic acids)
Aluminum, aluminium tris(acetylacetonate) and single acetyl acetone two (oacetic acid) aluminum etc..
The consumption of silanol condensation catalyst, based on the silicone modified polyester resin of 100 weight portions, control 0.01～
1 weight portion.If the consumption of silanol condensation catalyst is less than 0.01 weight portion, to the facilitation of silanol condensation reaction not
Substantially.If the consumption of silanol condensation catalyst is more than 1 weight portion, cause curing reaction too fast, ink composite is in printing
The rising of period viscosity is too fast, causes the reduction of printing quality.Too high silanol condensation catalyst consumption may also result in ink
Dyeing, reduction paint film endurance etc. affect.Certainly, for property optimum stable equilibrium, elect 0.05～0.5 weight portion as.
The polysiloxane defoamer that the present invention is used is selected from alkyl-modified polysiloxane defoamer and fluoroalkyl
At least one in modified polyorganosiloxanes defoamer.This two classes defoamer has below general formula：
In formula, R represents alkyl or fluorine
Alkyl.The main chain backbone of this two classes defoamer is Si-O-Si keys, similar to the Structure Mechanism of major ingredient, and cooperate lifting implementation ink
Excellent heat-resisting quantity.It is optimum according to property effect on usage amount ratio, the organosilicon modified polyester tree based on 100 weight portions
Fat, the consumption of polysiloxane defoamer is 0.1～4 weight portion.
The alkyl and/or aralkyl modified polysiloxane levelling agent that the present invention is used has following structure：
In formula, R represents alkyl and/or virtue
Alkyl.The main chain backbone of this kind of levelling agent is the Si-O-Si keys of excellent heat resistance, and side chain connection is alkyl or aralkyl, because
This has good yellowing resistance at high temperature.Based on the silicone modified polyester resin of 100 weight portions, alkyl and/or aralkyl
The consumption of base modified polyorganosiloxanes levelling agent is 0.1～4 weight portion.Organic silicon modified by polyether levelling agent and polyester modification have
Machine silicon levelling agent has the structure of similar alkyl and/or aralkyl modified polysiloxane levelling agent.Organic silicon modified by polyether
In substituting in levelling agent molecule in structure above, R group position is polyethers.Polyethers contains epoxy ethyl (EO) and/or epoxy
The chain link of propyl group (PO).Ehter bond (C-O-C) easy fracture at high temperature, so that the ink containing organic silicon modified by polyether levelling agent
Compositionss are easily turned to be yellow at high temperature.In polyester resin change properties of organic silicon levelling agent molecule, R group position is polyester in structural formula.Polyester
Modified organic silicon levelling agent has the thermostability better than organic silicon modified by polyether levelling agent, but still is not resistant to more than 250 DEG C
High temperature.Other levelling agents without organosilicon, such as polyacrylate levelling agent and fluorine-carbon modified polyacrylate stream
Flat agent, its main chain backbone are C-C keys, therefore heat-resisting quantity is not good.Therefore, reduce as far as possible in the present invention and adopt, if certainly
After creative means solve drawbacks described above, it is also possible to adopted according to effect.
Further, the solvent that the present invention is used is not particularly limited primarily as the disperse medium of ink, but preferably
Ketone, alcohols, esters, ether-ether class, alcohol ethers, fat hydrocarbon, aromatic hydrocarbon solvent and their mixture, and it is further excellent
Elect esters, ether-ether class, alcohol ethers, aromatic hydrocarbon solvent and their mixture as.Based on the organic-silicon-modified poly- of 100 weight portions
Ester resin, the consumption of solvent is 50～150 weight portions.It is for ink overall viscosity effect and the effect of printability, preferably molten
The consumption of agent causes the solid content of the high temperature resistant white glass ink composite of the present invention in the range of 60%～80%.Wherein,
As esters solvent, such as ethyl acetate, butyl acetate, gamma-butyrolacton, methyl lactate, ethyl lactate, succinic acid
Dimethyl ester, Glutaric Acid Dimethyl ester, adipic acid dimethyl ester, DBE, amyl valerate, isoamyl acetate, isobutyl acetate, butyl propionate,
Isopropyl isobutyrate, ethyl n-butyrate., butyl butyrate etc..
As solvent of ether ester type, such as ethylene glycol monomethyl ether acetate, ethyl cellosolve acetate, ethylene glycol monobutyl ether second
Acid esters, propylene glycol methyl ether acetate, propylene glycol monoethyl ether acetate, propandiol butyl ether acetass, diethylene glycol methyl ether acetic acid
Ester, diethylene glycol monoethyl ether acetass, diethylene glycol propyl ether acetass, diethylene glycol isopropyl ether acetass, diethylene glycol butyl ether second
Acid esters, diethylene glycol tertbutyl ether acetass, triethylene glycol methyl ether acetass, 3- methoxypropionates, 3- ethoxy-propionic acid second
Ester, 3- ethoxypropanoates etc..
As alcohol ethers solvent, such as glycol monoethyl ether, ethylene glycol monoethyl ether, ethylene glycol ether, ethylene glycol Dan Yi
Propyl ether, ethylene glycol monobutyl ether, ethylene glycol mono hexyl ether, glycol dimethyl ether, propylene glycol monomethyl ether, dihydroxypropane single-ether, the third two
Alcohol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol dimethyl ether, diethyl carbitol etc..
Present invention further propose that a kind of preparation method method of above-mentioned high temperature resistant ink, comprises the steps：
Before preparation, raw material can be obtained according to the reference in above-mentioned dispensing component；
S10, by the silicone modified polyester resin of 30～100 weight portions, the rutile titanium dioxide of 60～240 weight portions
After the mixing of powder, the aerosil of 0.5～10 weight portion and appropriate solvent, dispersion 10～60 minutes, form dispersion pulp at a high speed
Material；
Dispersed paste is reached less than 10 μm with grinder grinding distribution to fineness by S20 again, adds the organosilicon of surplus to change
The alkyl of property polyester resin, appropriate solvent, the polysiloxane defoamer of 0.1～4 weight portion and 0.1～4 weight portion and/
Or aralkyl modified polysiloxane levelling agent, stir, the host of ink is obtained；
S30, by the cross-linking agent of 1～30 weight portion, the silanol condensation catalyst of 0.01～1 weight portion and appropriate solvent
Mix homogeneously, is thus obtained the firming agent of ink；
In preparation process, the milling apparatus grinder of milled processed can be using three-roller, ball mill, horizontal sand mill, vertical
Formula sand mill, blue formula sand mill etc..Ink host obtained above and firming agent, can be kept separately in use, above-mentioned system
, from facilitating metering to consider, the proportioning of the host and firming agent of preferred ink is 100 for the ink host for obtaining and firming agent:5 or 100:
10；By the host and firming agent of the ink according to said ratio mix homogeneously after, glass is printed in by silk-screen printing technique
Glass base material, toasts 10～60 minutes through 150～200 DEG C and solidifies, just can form oil resistant layer of ink in substrate surface.Silk
Printed network yarn is not particularly limited, it is possible to use nylon grenadine, polyester grenadine and rustless steel grenadine；Purpose for accurate printing and
Effect, preferred polyester grenadine and rustless steel grenadine, grenadine mesh number are preferably 350～420 mesh.
In order to preferably help understand the present invention, and the excellent effect of the ink product to the present invention, below by way of many
Individual embodiment is illustrated：
Embodiment 1
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.5g(Evonik Degussa companies) and the gold of 50g
Red stone-type titanium dioxide(DuPont) mixes, with high speed dispersor (band diameter 3cm dispersion impellers) with
The rotating speed of 4000rpm/min disperses 30 minutes, forms dispersed slurry；
Then dispersed paste three-roller is ground to fineness and reaches less than 10 μm by S20, is supplemented with the CSH3000 trees of 14g
Fat, the defoamer BYK-077 (BYK companies) of 0.5g, the levelling agent BYK-322 (BYK companies) of 0.5g and the DBE solvents of 3g, stir
Mix uniform, the host of the high temperature resistant white glass ink composite of the present invention is obtained；
S30, by the MTMS of 3g, the dibutyl tin laurate Dabco T-12 (AIR of 0.03g
PRODUCTS companies) and 2.2g toluene mix homogeneously, be obtained the present invention high temperature resistant white glass ink composite solidification
Agent.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.
Embodiment 2
Silicone modified polyester resin CSH3000 in embodiment 1 is replaced with into silicone modified polyester resin SRE-906
(solid content is 60%, is provided by wealth and rank chemical raw material company limited of Guangzhou Dong) outward, in the same manner as example 1,
The high temperature resistant white glass ink composite of the present invention is prepared for, and carries out performance test.
Embodiment 3
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.8g(Evonik Degussa companies) and 50g's
Rutile type titanium dioxide(HUNTSMAN companies) mixes, with high speed dispersor (band diameter 3cm dispersions
Disk) disperseed 30 minutes with the rotating speed of 4000rpm/min, form dispersed paste；
Then dispersed paste three-roller is ground to fineness and reaches less than 10 μm by S20, is supplemented with the CSH3000 trees of 14g
The DBE solvents of fat, the levelling agent BYK-322 and 3g of defoamer BYK-077,0.5g of 0.5g, stir, and are obtained the present invention's
The host of high temperature resistant white glass ink composite；
S30, will be the toluene mixing of the methyl triacetoxysilane of 3g, the aluminium tris(acetylacetonate) of 0.03g and 2.21g equal
It is even, the firming agent of the high temperature resistant white glass ink composite of the present invention is obtained.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.
Embodiment 4
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.8g(Evonik Degussa companies) and 50g's
Rutile type titanium dioxide(HUNTSMAN companies) mixes, with high speed dispersor (band diameter 3cm dispersions
Disk) disperseed 30 minutes with the rotating speed of 4000rpm/min, form dispersed paste；
S20, then will form dispersed paste；Fineness is ground to three-roller and reaches less than 10 μm, be supplemented with 14g's
The DBE solvents of CSH3000 resins, the levelling agent BYK-322 and 3g of defoamer BYK-077,0.5g of 0.5g, stir, system
Obtain the host of high temperature resistant white glass ink composite of the invention；
S30, will be the toluene mixing of the methyl tributanoximo silane of 4g, the aluminium tris(acetylacetonate) of 0.06g and 1.18g equal
It is even, the firming agent of the high temperature resistant white glass ink composite of the present invention is obtained.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.
Embodiment 5
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.8g(Evonik Degussa companies) and 50g's
Rutile type titanium dioxide(HUNTSMAN companies) mixes, with high speed dispersor (band diameter 3cm dispersions
Disk) disperseed 30 minutes with the rotating speed of 4000rpm/min, form dispersed paste；
S20, then will form dispersed paste；Fineness is ground to three-roller and reaches less than 10 μm, be supplemented with 14g's
The DBE solvents of CSH3000 resins, the levelling agent BYK-322 and 3g of defoamer BYK-077,0.5g of 0.5g, stir, system
Obtain the host of high temperature resistant white glass ink composite of the invention；
S30, by polysilazane DURAZANE1500SC (AZ Electronic Materials companies), the 0.5g of 1.2g
Epoxy silane coupling(Evonik Degussa companies), the three (levulinics of 0.03g
Ketone) aluminum and 3.51g toluene mix homogeneously, the firming agent of the high temperature resistant white glass ink composite of the present invention is obtained.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.Test result is reported in Table 2 below.
Embodiment 6
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.8g(Evonik Degussa companies) and 50g's
Rutile type titanium dioxide(HUNTSMAN companies) mixes, with high speed dispersor (band diameter 3cm dispersions
Disk) disperseed 30 minutes with the rotating speed of 4000rpm/min, form dispersed paste；
S20, then will form dispersed paste three-roller and be ground to fineness and reach less than 10 μm, be supplemented with 14g's
CSH3000 resins, height normal-butyl etherified amino resins CYMEL1156 (CYTEC companies) of 0.75g, the defoamer of 0.5g
The DBE solvents of the levelling agent BYK-322 and 3g of BYK-077,0.5g, stir, and the high temperature resistant white glass of the present invention is obtained
The host of ink composite；
S30, by the epoxy silane coupling of 3g(Evonik Degussa companies),
The toluene mix homogeneously of the aluminium tris(acetylacetonate) and 2.22g of 0.06g, is obtained the high temperature resistant white glass ink combination of the present invention
The firming agent of thing.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.
Embodiment 7
Defoamer BYK-077 in embodiment 4 is replaced with into BYK-066N (BYK companies), with 4 identical side of example
Formula, is prepared for the high temperature resistant white glass ink composite of the present invention, and carries out performance test.
Comparative example 1
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.8g(Evonik Degussa companies) and 50g's
Rutile type titanium dioxide(HUNTSMAN companies) mixes, with high speed dispersor (band diameter 3cm dispersions
Disk) disperse 30 minutes to form dispersed paste with the rotating speed of 4000rpm/min；
S20, then will form dispersed paste three-roller and be ground to fineness and reach less than 10 μm, be supplemented with 14g's
The DBE solvents of CSH3000 resins, the levelling agent BYK-322 and 3g of defoamer BYK-077,0.5g of 0.5g, stir, system
Obtain the host of white glass ink composite；
S30, by the amino silicane coupling agent of 2.0g(Evonik Degussa companies),
The toluene mix homogeneously of the aluminium tris(acetylacetonate) and 3.18g of 0.06g, is obtained the firming agent of white glass ink composite.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.
Comparative example 2
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.8g(Evonik Degussa companies) and 50g's
Rutile type titanium dioxide(HUNTSMAN companies) mixes, with high speed dispersor (band diameter 3cm dispersions
Disk) disperse 30 minutes to form dispersed paste with the rotating speed of 4000rpm/min；
S20, then will form dispersed paste three-roller and be ground to fineness and reach less than 10 μm, be supplemented with 14g's
CSH3000 resins, the high imino group resin CYMEL325 (CYTEC companies) of 0.75g, defoamer BYK-077,0.5g of 0.5g
The DBE solvents of levelling agent BYK-322 and 3g, stir, and the host of white glass ink composite is obtained；
S30, will be the toluene mixing of the MTMS of 3g, the aluminium tris(acetylacetonate) of 0.06g and 2.22g equal
It is even, the firming agent of white glass ink composite is obtained.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.
Comparative example 3
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.8g(Evonik Degussa companies) and 50g's
Rutile type titanium dioxide(HUNTSMAN companies) mixes, with high speed dispersor (band diameter 3cm dispersions
Disk) disperseed 30 minutes with the rotating speed of 4000rpm/min, form dispersed paste；
S20, then will form dispersed paste three-roller and be ground to fineness and reach less than 10 μm, be supplemented with 14g's
The DBE solvents of CSH3000 resins, the levelling agent BYK-322 and 3g of defoamer BYK-077,0.5g of 0.5g, stir, system
Obtain the host of white glass ink composite；
S30, by the blocked polyisocyanate firming agent of 2.0gSN (Bayer companies),
The epoxy silane coupling of 0.5g(Evonik Degussa companies), the three (second of 0.06g
Acyl acetone) aluminum and 2.68g toluene mix homogeneously, the firming agent of white glass ink composite is obtained.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.
Comparative example 4
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.8g(Evonik Degussa companies) and 50g's
Rutile type titanium dioxide(HUNTSMAN companies) mixes, with high speed dispersor (band diameter 3cm dispersions
Disk) disperseed 30 minutes with the rotating speed of 4000rpm/min, form dispersed paste；
S20, then will form dispersed paste three-roller and be ground to fineness and reach less than 10 μm, be supplemented with 14g's
The fluorine-carbon modified polyacrylate levelling agent Afcona-3777s of CSH3000 resins, defoamer BYK-077,0.5g of 0.5g
(Afcona companies) and the DBE solvents of 3g, stir, and the host of white glass ink composite is obtained；
S30, will be the toluene mixing of the methyl tributanoximo silane of 4g, the aluminium tris(acetylacetonate) of 0.06g and 1.18g equal
It is even, the firming agent of white glass ink composite is obtained.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.
Comparative example 5
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.8g(Evonik Degussa companies) and 50g's
Rutile type titanium dioxide(HUNTSMAN companies) mixes, with high speed dispersor (band diameter 3cm dispersions
Disk) disperseed 30 minutes with the rotating speed of 4000rpm/min, form dispersed paste；
S20, then will form dispersed paste three-roller and be ground to fineness and reach less than 10 μm, be supplemented with 14g's
The polyether polyester modification by copolymerization polysiloxane levelling agent of CSH3000 resins, defoamer BYK-077,0.5g of 0.5gThe DBE solvents of (Guangzhou Si Luoke Chemical Co., Ltd) and 3g, stir, and white glass ink is obtained
The host of compositionss；
S30, will be the toluene mixing of the methyl tributanoximo silane of 4g, the aluminium tris(acetylacetonate) of 0.06g and 1.18g equal
It is even, the firming agent of white glass ink composite is obtained.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.
Comparative example 6
S10, by the silicone modified polyester resin CSH3000 of 36g, (solid content is 60%, by Shenzhen's wound generation perseverance trade
Company limited provide), the aerosil of 0.8g(Evonik Degussa companies) and 50g's
Rutile type titanium dioxide(HUNTSMAN companies) mixes, with high speed dispersor (band diameter 3cm dispersions
Disk) disperse 30 minutes to form dispersed paste with the rotating speed of 4000rpm/min；
S20, then will form dispersed paste three-roller and be ground to fineness and reach less than 10 μm, be supplemented with 14g's
CSH3000 resins, non-silicon class defoamer Afcona-2720 (Afcona companies) of 0.5g, the levelling agent BYK-322 and 3g of 0.5g
DBE solvents, stir, the host of white glass ink composite be obtained；
S30, will be the toluene mixing of the methyl tributanoximo silane of 4g, the aluminium tris(acetylacetonate) of 0.06g and 1.18g equal
It is even, the firming agent of white glass ink composite is obtained.
The host and firming agent of ink are pressed into 100:5 ratio mix homogeneously, makes glass lens sample, and carries out performance
Test.
By glass lens sample obtained in the various embodiments described above and comparative example, carry out performance test bag and include：
(1) pencil hardness test：According to《GB/T 6739-2006 paint and varnish pencils method determines hardness of paint film》Test
The pencil hardness of paint film.
(2) adhesive force test：According to《The cross cut test of GB/T 9286-1998 paint and varnish paint films》Test paint film
Adhesive force.
(3) resistance to boiling water test：Glass lens sample is placed in into boiling test case, in 100 DEG C of deionized waters at ambient pressure
Boil 1 hour, the change of paint film appearance is observed in taking-up after drying 24 hours, and tests the adhesive force of paint film.
(4) resistance to butanone test：Full chemical pure butanone is dipped in white softness non-dust cloth, applies 500g power, on paint film back and forth
Wipe 50 times, come and go as once, whether observation non-dust cloth dyes, whether paint film is damaged, come off, fade.
(5) resistance to inorganic developer solution test：Glass lens sample is soaked in 1000 seconds in inorganic developer solution, taking-up is dried
The change of paint film appearance is observed after 24 hours, and tests the adhesive force of paint film.
(6) stripper solution of resistance to photoresist test：Glass lens sample is soaked in 1000 seconds in photoresist stripper solution, is taken out
The change of paint film appearance is observed after drying 24 hours, and tests the adhesive force of paint film.
(7) resistance to ITO etching solutions test：Glass lens sample is soaked in 1000 seconds in ITO etching solutions, taking-up dries 24
The change of paint film appearance is observed after hour, and tests the adhesive force of paint film.
(8) high temperature resistant test：Glass lens sample is put in 300 DEG C of air dry oven and toasts 30min, take out nature
The change of paint film appearance is observed in cooling after 2 hours, and tests the adhesive force of paint film.
(8) high-temp resisting high-humidity resisting test：Glass lens sample is placed in into the test environment that temperature is 60 DEG C, humidity is 95%RH
The change of paint film appearance is observed in middle storage 120 hours, taking-up after drying 24 hours, and tests the adhesive force of paint film.
(9) high-low temperature resistant shock-testing：Glass lens sample is put in thermal shock test chamber carry out it is cold such as table 1 below
Thermal shock test, repeats 40 cycles, observes the change of paint film appearance, and test the adhesive force of paint film after taking-up.
| Temperature | 80℃ | Room temperature | -20℃ | Room temperature |
| Time | 2 hours | 0.5 hour | 2 hours | 0.5 hour |
(10) salt spray resistance test：With reference to《The measure of the resistance to neutral salt spray performance of GB/T 1771-2007 paint and varnish》, it is right
Glass lens sample carries out the neutral salt spray test of 120 hours, and the change of paint film appearance is observed in taking-up after drying 24 hours, and is surveyed
The adhesive force of examination paint film.
Test result such as table 2 below：
From table 2 it can be seen that the high temperature resistant white glass ink composite of the present invention, with splendid to glass baseplate
Adhesive force and good chemical-resistant, it is often more important that, with the resisting high-temperature yellowing for significantly improving.Comparative example 1 is used
Amino silicane coupling agent, comparative example 2 and comparative example 3 have used high imino group resin CYMEL325 and enclosed type polyisocyanic acid respectively
Ester firming agentUsed as cross-linking agent, comparative example 4 has used fluorine-carbon modified polyacrylate stream to SN
Flat agent Afcona-3777s, comparative example 5 have used polyether polyester modification by copolymerization polysiloxane levelling agent
Comparative example 6 has used non-silicon class defoamer Afcona-2720, causes white ink composition yellowing resistance at high temperature to be sent out
It is raw substantially to deteriorate.And the performance of each side of the ink product obtained by preparing in the present invention, especially thermostability and anti-yellowing property
Compare existing ink to be obviously improved.
The present invention further also proposes a kind of OGS contact panels that gained is prepared using above-mentioned high temperature resistant ink.Using this
Invention above-mentioned high temperature resistant ink, by ink host and firming agent substep prepare, finally carry out again it is mixing cured, then by this
The high temperature resistant ink of bright middle preparation is used in OGS processing procedures, and final acquisition is obtained by prepared by adopting the high temperature resistant ink of the present invention
OGS contact panels；Process is simple, and can substantially ensure that stable in properties, the effect of ink reach most preferably.And adopt and send out
OGS contact panels prepared by bright high temperature resistant ink, after the techniques such as follow-up high temperature, plated film, etching, ink property is not sent out
It is raw to change, nor can turn yellow；Display effect is more preferable.
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., all should be included within protection scope of the present invention.
Claims (7)
1. a kind of high temperature resistant ink, it is characterised in that be grouped into by each group of following mass parts：
100 parts of organic-silicon-modified resin, 60～240 parts of titanium dioxide, 0.5～10 part of aerosil, 1～30 part of cross-linking agent,
0.01～1 part of silanol condensation catalyst, 0.1～4 part of polysiloxane defoamer, alkyl and/or aralkyl modified poly- have
0.1～4 part of organic siloxane levelling agent, 50～150 parts of solvent；The organic-silicon-modified resin accounts for the part by weight of high temperature resistant ink
For 20～40%；
Wherein, contain at least one reactive silicon group in the organic-silicon-modified molecular resin, the reactive silicon group has
Following group：
Wherein,
R in formula1And R2It is 7～20 for alkyl, the aryl that carbon number is 6～20 or carbon number that carbon number is 1～20
Aralkyl；X is hydroxyl or hydrolization group；M is 1～3 integer, and n is 1～2 integer, and the hydrolysising group is that hydrogen is former
Son, halogen atom, alkoxyl, acyloxy, ketoxime base；
The cross-linking agent is silane crosslinker, epoxy silane coupling, amino resins, at least one in polysilazane；
The silane crosslinker includes following structure：RnSiX4-n, n is 0～2 integer；In formula R be from carbon number be 1～10
Alkyl, the aryl that carbon number is 6～10 or aralkyl that carbon number is 7～10；X is alkoxyl, acyloxy, ketoxime base
And at least one in alkenyloxy group.
2. high temperature resistant ink as claimed in claim 1, it is characterised in that the epoxy silane coupling is γ-(2,3- rings
Oxygen propoxyl group) propyl trimethoxy silicane, γ-(2,3- glycidoxies) propyl-triethoxysilicane, γ-(2,3- epoxies third
Epoxide) hydroxypropyl methyl dimethoxysilane, the one kind or many in γ-(2,3- glycidoxies) hydroxypropyl methyl diethoxy silane
The mixture planted.
3. high temperature resistant ink as claimed in claim 1, it is characterised in that the amino resins are highly methyl etherified amino tree
In the mixed etherified amino resins of fat, height butyl etherified amino resins, highly etherification benzene substituted amino resins and height etherificate one
Plant or various mixture.
4. high temperature resistant ink as claimed in claim 1, it is characterised in that the polysiloxane defoamer is alkyl-modified
At least one in polysiloxane defoamer and fluoroalkyl polysiloxane defoamer；
And/or,
The silanol condensation catalyst be mineral acid, inorganic base, organic acid, organic amine compound, in organo-metallic compound
At least one；
And/or,
Rutile type titanium dioxide of the titanium dioxide for 0.15～0.50 μm of particle diameter.
5. the preparation method of the high temperature resistant ink as described in any one of Claims 1-4, it is characterised in that comprise the steps：
By 30～100 parts in the silicone modified polyester resin of 100 weight portion of raw material and Rutile type titanium dioxide, gas phase dioxy
After SiClx is mixed with partial solvent, dispersed formation dispersed paste；
The dispersed paste is ground and is dispersed to fineness and is reached after less than 10 μm, add remaining organosilicon modified polyester tree
Fat, polysiloxane defoamer, alkyl and/or aralkyl modified polysiloxane levelling agent and partial solvent, uniformly
Mix to obtain ink host；
By cross-linking agent, silanol condensation catalyst and residual solvent mix homogeneously, ink solidification agent is obtained.
6. the preparation method of high temperature resistant ink as claimed in claim 5, it is characterised in that the cross-linking agent, silanol contract
Catalyst and residual solvent mix homogeneously are closed, is also included after obtaining ink solidification agent step：
After the ink host is uniformly mixed with ink solidification agent, after being printed on base material by silk screen printing, solidified
Process.
7. a kind of OGS contact panels, it is characterised in that include the high temperature resistant ink as described in any one of claim 1 to 5.
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| CN105062203B (en) * | 2015-08-31 | 2018-05-25 | 洋紫荆油墨(中山)有限公司 | A kind of water resistance one-component glass ink and preparation method thereof |
| CN105459655B (en) * | 2015-11-30 | 2018-03-09 | 广东星弛光电科技有限公司 | A kind of printing process of mobile phone faceplate base |
| CN105238133B (en) * | 2015-11-30 | 2017-10-17 | 佛山市高明绿色德化工有限公司 | A kind of ink and its application method applied on coated glass |
| CN105907289B (en) * | 2016-06-23 | 2019-06-18 | 张家港康得新光电材料有限公司 | Thermal transfer protecting layer compositions, heat transfer film and preparation method thereof |
| CN106046926A (en) * | 2016-07-08 | 2016-10-26 | 广东顺德晶纬玻璃制品有限公司 | High-temperature-resistant transparent stereoscopic printing ink and method for preparing same |
| US10593439B2 (en) * | 2016-10-21 | 2020-03-17 | Dupont Electronics, Inc. | Conductive paste composition and semiconductor devices made therewith |
| CN107652766A (en) * | 2017-11-17 | 2018-02-02 | 安徽银兔装饰材料有限公司 | High temperature resistant ink and preparation method thereof |
| CN107652750A (en) * | 2017-11-17 | 2018-02-02 | 安徽银兔装饰材料有限公司 | Ink curing agent and preparation method thereof |
| CN107880640A (en) * | 2017-12-21 | 2018-04-06 | 刘辉 | A kind of high performance heat resistant ink |
| CN108384314A (en) * | 2018-03-21 | 2018-08-10 | 湖北中烟工业有限责任公司 | A kind of UV gravures snowflake printing ink |
| CN110305529A (en) * | 2019-07-29 | 2019-10-08 | 佛山市高明绿色德化工有限公司 | A kind of high temperature resistant ink for devitrified glass and preparation method thereof, application method |
| CN113372758A (en) * | 2021-08-12 | 2021-09-10 | 北京康美特科技股份有限公司 | White organic silicon printing ink, reflecting layer, backlight substrate and backlight module |
| CN115595015B (en) * | 2022-07-05 | 2023-11-14 | 佛山市儒林化工有限公司 | High-temperature-resistant super-bright extra-white ink and preparation method thereof |
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| US7438958B2 (en) * | 2002-11-01 | 2008-10-21 | Mitsui Chemicals, Inc. | Sealant composition for liquid crystal and process for producing liquid-crystal display panel with the same |
| TWM441133U (en) * | 2012-05-10 | 2012-11-11 | Mortech Corp | A reflecting film preventing light leakage, and a led light bar and a LCD's backlight using the same |
| CN103319949B (en) * | 2013-06-18 | 2014-10-22 | 厦门市豪尔新材料有限公司 | OGS (One Glass Solution) glass protecting ink as well as preparation method and application thereof |
| CN103436094B (en) * | 2013-08-27 | 2015-10-28 | 华南理工大学 | High temperature resistant touch screen ink of a kind of thermoset and preparation method thereof |
| CN103881474A (en) * | 2014-02-26 | 2014-06-25 | 金甲化工企业(中山)有限公司 | High-temperature-resistant yellowing-free ink |
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