CN104151925A - High-temperature-resistant ink, preparation method thereof and OGS touch panel - Google Patents
High-temperature-resistant ink, preparation method thereof and OGS touch panel Download PDFInfo
- Publication number
- CN104151925A CN104151925A CN201410351240.6A CN201410351240A CN104151925A CN 104151925 A CN104151925 A CN 104151925A CN 201410351240 A CN201410351240 A CN 201410351240A CN 104151925 A CN104151925 A CN 104151925A
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- Prior art keywords
- agent
- parts
- ink
- resin
- high temperature
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- 238000002360 preparation method Methods 0.000 title description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 105
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- 239000011347 resin Substances 0.000 claims abstract description 40
- 229920005989 resin Polymers 0.000 claims abstract description 39
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 28
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 27
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 25
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- 239000004408 titanium dioxide Substances 0.000 claims abstract description 23
- -1 polysiloxane Polymers 0.000 claims abstract description 21
- 239000003054 catalyst Substances 0.000 claims abstract description 20
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 20
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 17
- 238000009833 condensation Methods 0.000 claims abstract description 13
- 230000005494 condensation Effects 0.000 claims abstract description 13
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 65
- 239000000203 mixture Substances 0.000 claims description 51
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- 238000002156 mixing Methods 0.000 claims description 32
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- 238000000227 grinding Methods 0.000 claims description 16
- 125000003710 aryl alkyl group Chemical group 0.000 claims description 15
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- 125000003118 aryl group Chemical group 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
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- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 2
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- 125000001183 hydrocarbyl group Chemical group 0.000 description 4
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 4
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 3
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 description 3
- 125000004429 atom Chemical group 0.000 description 3
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XLLIQLLCWZCATF-UHFFFAOYSA-N ethylene glycol monomethyl ether acetate Natural products COCCOC(C)=O XLLIQLLCWZCATF-UHFFFAOYSA-N 0.000 description 3
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 3
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 3
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
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- 239000004677 Nylon Substances 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
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- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
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- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical compound CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 1
- 230000009974 thixotropic effect Effects 0.000 description 1
- KSBAEPSJVUENNK-UHFFFAOYSA-L tin(ii) 2-ethylhexanoate Chemical compound [Sn+2].CCCCC(CC)C([O-])=O.CCCCC(CC)C([O-])=O KSBAEPSJVUENNK-UHFFFAOYSA-L 0.000 description 1
- YZVRVDPMGYFCGL-UHFFFAOYSA-N triacetyloxysilyl acetate Chemical compound CC(=O)O[Si](OC(C)=O)(OC(C)=O)OC(C)=O YZVRVDPMGYFCGL-UHFFFAOYSA-N 0.000 description 1
- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 description 1
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- 150000003755 zirconium compounds Chemical class 0.000 description 1
Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention provides high-temperature-resistant ink. The high-temperature-resistant ink comprises the following components: 100 parts of organosilicone-modified resin, 60-240 parts of titanium dioxide powder, 0.5-10 parts of fumed silica, 1-30 parts of crosslinking agent, 0.01-1 part of silanol condensation catalyst, 0.1-4 parts of polysiloxane defoaming agent, 0.1-4 parts of alkyl and/or aralkyl-modified polyorganosiloxane leveling agent and 50-150 parts of solvent. According to the high-temperature-resistant ink disclosed by the invention, since organosilicone-modified resin is adopted as a main component and functional additives such as the specific crosslinking agent, the silanol condensation catalyst, the defoaming agent and the leveling agent, are mixed to jointly improve the performances, such as high temperature resistance, resistance to yellowing, stability and the like of an ink product and thus a white glass ink product with excellent high temperature resistance and chemical resistance is obtained.
Description
Technical Field
The invention belongs to the technical field of printing ink for touch panels, and particularly relates to high-temperature-resistant printing ink, a preparation method of the high-temperature-resistant printing ink and an OGS touch panel.
Background
In the existing OGS (One Glass Solution, integrated touch) touch panel process, high-temperature-resistant ink is firstly required to be printed on an ITO (indium tin oxide) substrate, the hardness and chemical resistance of the surface are controlled, and the conductive silver paste, an ITO coating, photoresist printing, exposure, development, ITO film etching, photoresist stripping and the like are effectively protected in the subsequent process; and then can control adhesive force, hardness and demolding time, can promote the yields by a wide margin. In the above process, the high temperature resistant ink is printed first and then subjected to subsequent treatments such as high temperature environment, developing solution, ITO etching solution, etc. The main material of the existing high-temperature resistant ink is the organosilicon modified epoxy resin with high and low temperature resistance, weather aging resistance and high insulation strength; however, due to the molecular structure of the main materials of the ink products, the ink products are easy to turn yellow in the high-temperature treatment within the range of 250-300 ℃, and the display effect of the OGS touch panel is seriously influenced; and the functional auxiliary agent is selected aiming at the main material, and the printing ink cannot have good effects and functions in the aspects of temperature resistance and yellowing resistance due to the consideration of overall stability, viscosity, hardness and the like.
Disclosure of Invention
The embodiment of the invention aims to overcome the defects in the prior art and provide the high-temperature-resistant ink which has better high-temperature-resistant performance and does not turn yellow within the range of 250-300 ℃.
In order to achieve the above purpose, the technical solution of the embodiment of the present invention is as follows:
the high-temperature-resistant ink comprises the following components in parts by mass:
100 parts of organic silicon modified resin, 60-240 parts of titanium dioxide, 0.5-10 parts of fumed silica, 1-30 parts of a cross-linking agent, 0.01-1 part of silanol condensation catalyst, 0.1-4 parts of a polysiloxane defoaming agent, 0.1-4 parts of an alkyl and/or aralkyl modified polysiloxane flatting agent and 50-150 parts of a solvent.
According to the high-temperature-resistant ink product, the organic silicon modified resin is used as a main material, and the special cross-linking agent, the silanol condensation catalyst, the defoaming agent, the flatting agent and other functional auxiliaries are matched to improve the effects of high temperature resistance, yellowing resistance, stability and the like of the ink product, so that the white glass ink product with excellent high-temperature resistance and chemical resistance is obtained.
The invention further provides a preparation method of the high-temperature-resistant ink, which comprises the following steps:
mixing 30-100 parts by weight of raw materials in 100 parts by weight of organic silicon modified polyester resin with rutile titanium dioxide and a part of solvent for fumed silica, and uniformly dispersing to form dispersed slurry;
grinding and dispersing the dispersed slurry until the fineness is below 10 mu m, adding the rest organic silicon modified polyester resin, the organic polysiloxane defoaming agent, the alkyl and/or aralkyl modified organic polysiloxane flatting agent and part of solvent, and uniformly mixing to obtain the main printing ink agent;
and uniformly mixing the cross-linking agent, the silanol condensation catalyst and the residual solvent to obtain the ink curing agent.
The invention further provides an OGS touch panel prepared by adopting the high-temperature-resistant ink.
The high-temperature-resistant ink is prepared by distributing the main ink agent and the curing agent, and finally, is mixed and cured, has simple process, and can maximally ensure the stable property and the optimal effect of the ink. The OGS touch panel prepared by the high-temperature-resistant ink has the advantages that the ink property is not changed and is not yellowed after subsequent processes such as high temperature, film coating, etching and the like; the display effect is better.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides high-temperature-resistant ink which comprises the following components in parts by mass:
100 parts of organic silicon modified resin, 60-240 parts of titanium dioxide, 0.5-10 parts of fumed silica, 1-30 parts of a cross-linking agent, 0.01-1 part of silanol condensation catalyst, 0.1-4 parts of a polysiloxane defoaming agent, 0.1-4 parts of an alkyl and/or aralkyl modified polysiloxane flatting agent and 50-150 parts of a solvent.
In the high-temperature resistant ink product, organic silicon modified resin is used as a main material, and a specific cross-linking agent, a silanol condensation catalyst, a defoaming agent, a leveling agent and other functional auxiliaries are matched to improve the effects of high temperature resistance, yellowing resistance, stability and the like of the ink product, so that a white glass ink product with excellent high-temperature resistance and chemical resistance is obtained.
Wherein the organosilicon-modified resin contains at least 1 reactive silicon group in the molecule, and the reactive silicon groups can form a siloxane bond to crosslink with each other. The reactive silicon group has a group represented by the following general formula:
in the formula, R1And R2Each independently represents an alkyl group having 1 to 20 carbon atoms, an aryl group having 6 to 20 carbon atoms or an aralkyl group having 7 to 20 carbon atoms. When the reactive silicon group has plural R1Or R2When R is plural1R between or more than2The same or different. X represents a hydroxyl group or a hydrolyzable group. When the reactive silicon group has a plurality of xs, the plurality of xs may be the same or different. In addition, m represents an integer of 1 to 3, and n represents an integer of 1 to 2.
Wherein, when X is a hydrolyzable group, it can be selected from hydrogen atom, halogen atom, alkoxy, acyloxy, ketoxime group, etc.; among them, alkoxy groups are preferable from the viewpoint of keeping the mildness of the hydrolysis reaction.
In the silicon-modified resin of the present invention, in order to satisfy the effect of increasing the crosslink density of the cured paint film, it is preferable that the molecule contains 2 or more reactive silicon groups.
The organic silicon modified resin as the main material in the ink is an organic-inorganic hybrid high polymer material with Si-O-Si bonds as a main chain and organic groups on side chains. The Si-O bond has a high bond energy (443.7kJ/mol), higher than the bond energy (347.4kJ/mol) of the C-C bond in the conventional organic resin, and good thermal stability. The relative electronegativity difference between Si atoms and O atoms in Si-O bonds is large, so that the Si-O bonds have large polarity and high ionization tendency (51%), have dipole induction influence on hydrocarbon groups connected on the Si atoms, and improve the stability of the hydrocarbon groups connected with Si on oxidation, namely the Si-O-Si bonds play a certain role in shielding the oxidation of the hydrocarbon groups. The Si-C bond energy is lower than that of the C-C bond, but a d pi-p pi complex bond can be formed in the Si-C bond, so that the energy of the system is reduced, and the thermal oxidation stability of the resin is improved. C-C bond of common organic resin is easily broken into low molecular substance by thermal oxidation, and hydrocarbon group connected with Si atom is heated and oxidized to generate highly cross-linked more stable Si-O-Si bond which can prevent the breakage and degradation of main chain. All the factors enable the organic silicon modified resin to have excellent thermal oxidation stability, and after the organic silicon modified resin is heated for 24 hours at the temperature of 250 ℃, the weight loss of the organic silicon modified resin is only 2-8%. The silicone-modified resin also has outstanding weatherability and resistance to yellowing even under intense ultraviolet irradiation. The main material organic silicon modified polyester resin adopted by the invention generates condensation reaction between different reactive silicon groups or between the reactive silicon groups and a cross-linking agent containing active Si through the reactive silicon groups to remove water, alcohol, carboxylic acid, ketone, ketoxime and other small molecules and form Si-O-Si bonds. As a result of the formation of Si-O-Si bonds, the ink composition has excellent high temperature resistance.
The organic silicon modified polyester resin adopted in the invention is a copolymer which is formed by connecting the polyester resin on the tail end or the side chain of the main chain of the polyorganosiloxane through polycondensation to form a block, graft or interpenetrating network structure. Has the advantages of good adhesion of polyester resin and good chemical resistance, has the characteristics of excellent thermal oxidation resistance and weather resistance of organic silicon resin, and can be cured at a lower temperature (less than 200 ℃).
In the high-temperature resistant ink product, according to the requirements of performance tests and use effects, the weight proportion of the organic silicon modified polyester resin in the high-temperature resistant ink is controlled to be 20-40%; if the content of the silicone-modified polyester resin is less than 20 parts by weight, the mechanical strength of a paint film formed after the ink composition is cured becomes poor. If the content of the organic silicon modified polyester resin is higher than 40 parts by weight, the titanium dioxide needs to be compressed in the ink composition, so that the content is relatively low, and the covering power of a paint film formed after final curing is reduced. Based on the situation, the weight proportion of the ink in the high-temperature resistant ink is controlled to be 25-35% most preferably, so that various performances tend to be balanced and stable, and the overall performance of an ink product is further ensured.
Further, in the above embodiment, the titanium dioxide used in the present invention is rutile titanium dioxide, and the particle size is controlled within the range of 0.15 to 0.50 μm; the titanium dioxide of the type can be used as a whitening agent to improve the color effect, has stable crystal lattices in the particle size and type, has stronger reinforcing, anti-aging and filling functions after being added, and improves the covering power. And the titanium dioxide belongs to hydrophilic substances, but the hygroscopicity of the titanium dioxide is not strong, so that the surface property of the ink product is facilitated. The dosage is based on 100 weight parts of organic silicon modified polyester resin, and the dosage of rutile type titanium dioxide is selected from 60-240 weight parts; the optimal rutile titanium dioxide is 100-200 parts by weight, so that the balance of the mechanical property and the comprehensive property of the covering power of the whole paint film of the ink is optimal.
Further, after the fumed silica is added on the basis of the main materials, the special chemical inertia and the special thixotropic property of the fumed silica can be used for synergistically facilitating the control of ink adhesion, rheological property and thixotropy; because the high-temperature resistant ink has the processes of high temperature, etching and the like in the subsequent process of the OGS touch panel, under the condition of very large environmental change difference, the performance of the high-temperature resistant ink is necessarily prevented from mutating, and the addition of the fumed silica can ensure the moderate capability of the ink in the aspects of fluidity and the like under the condition of great change. In the present invention, the fumed silica is at least one of hydrophilic type fumed silica or hydrophobic type fumed silica. And the amount of fumed silica is 0.5 to 10 parts by weight based on 100 parts by weight of the silicone-modified polyester resin for the balance stability of the properties thereof; the optimal weight is 1 to 5 parts.
The crosslinking agent used in the present invention is at least one selected from the group consisting of a silane crosslinking agent, an epoxy silane coupling agent, an amino resin, and a polysilazane.
The silane cross-linking agent has the following structural formula: rnSiX4-n(n is an integer of 0 to 2). R represents an alkyl group having 1 to 10 carbon atoms, an aryl group having 6 to 10 carbon atoms or an aralkyl group having 7 to 10 carbon atoms; such as methyl, ethyl, propyl, isopropyl, butyl, isobutyl, octyl, phenyl, methyl, isobutyl, octyl, and octyl,P-methylphenyl, benzyl, and the like. When the silane crosslinking agent has two R groups in the molecule, the R groups may be the same or different. X represents at least one selected from the group consisting of an alkoxy group, an acyloxy group, a ketoximino group and an alkenyloxy group. From the viewpoint of availability of raw materials, X is preferably at least one of a methoxy group, an ethoxy group, an acetoxy group, a butanone oxime group, and an isopropenoxy group.
The silane cross-linking agent adopted by the invention is matched with the main material adopted in the printing ink, and when the silane cross-linking agent in the printing ink composition meets water vapor, alkoxy, acyloxy, ketoxime or alkenyloxy of the silane cross-linking agent can be hydrolyzed to form silanol groups which can be subjected to condensation reaction with reactive silicon groups on the organic silicon modified polyester resin, so that a Si-O-Si bond network with excellent heat resistance is formed; finally, the modified polyester film interacts with the main material of the organic silicon modified polyester to form a cross-linked structure, so that the heat resistance of the film is improved. The silane crosslinking agent having the above structure may be selected from methyltrimethoxysilane, methyltriethoxysilane, propyltrimethoxysilane, propyltriethoxysilane, isobutyltrimethoxysilane, isobutyltriethoxysilane, octyltrimethoxysilane, octyltriethoxysilane, phenyltrimethoxysilane, phenyltriethoxysilane, methyl orthosilicate, ethyl orthosilicate, n-propyl orthosilicate, methyltriacetoxysilane, ethyltriacetoxysilane, propyltriacetoxysilane, phenyltriacetoxysilane, dimethyldiacetoxysilane, tetraacetoxysilane, methyltributanonoximosilane, dimethyldibutyloximosilane, tetrabutoximosilane, phenyltributonoximosilane, methyltris (isopropenoxy) silane, dimethyldi (isopropenoxy) silane, tetra (isopropenoxy) silane, n-propyl triethoxysilane, iso-triethoxysilane, phenyltriethoxysilane, n-propyl orthosilicate, phenyltriacetoxysilane, dimethyldiacetoxy silane, and a mixture thereof, Phenyltri (isopropenyloxy) silane, and the like.
The epoxy silane coupling agent of the present invention may be one or more selected from the group consisting of γ - (2, 3-epoxypropoxy) propyltrimethoxysilane, γ - (2, 3-epoxypropoxy) propyltriethoxysilane, γ - (2, 3-epoxypropoxy) propylmethyldimethoxysilane, and γ - (2, 3-epoxypropoxy) propylmethyldiethoxysilane. This type of epoxy silane coupling agent and silane crosslinking agent are not combined with the main material in the same manner, but similar effects can be achieved. The alkoxy group of the epoxy silane coupling agent can also react with the reactive silicon group of the organic silicon modified polyester resin to form an Si-O-Si bond with excellent heat resistance; the epoxy group of the epoxy silane coupling agent is difficult to participate in the reaction and open the ring at the temperature of below 200 ℃, and when the temperature exceeds 200 ℃, the epoxy group can react with the silanol group on the reactive silicon group of the organic silicon modified polyester resin to form an Si-O-C bond with good heat resistance.
Among them, the amino resin used in the present invention is preferably one or a mixture of more of a highly methylated amino resin, a highly butyl-etherified amino resin, a highly etherified phenylated amino resin and a highly etherified mixed etherified amino resin. The highly methyl etherified amino resin, the highly butyl etherified amino resin and the highly etherified mixed etherified amino resin in the amino resins have the following structural general formulas:
the highly etherified phenylamino resin has the following general formula:
r in the structural formula represents methyl, n-butyl or isobutyl, and a plurality of R can be the same or different; r3Represents a H atom or CH2OH group (hydroxymethyl). Alkoxy groups (OR groups) and hydroxymethyl groups (CH) in these amino resins2OH group) can undergo a condensation reaction with the reactive silicon group of the silicone-modified polyester resin to form a Si-O-C bond having good heat resistance.
The last polysilazane in the crosslinker of the invention has the following structure:wherein R is H or alkyl, and R's may be the same or different. Polysilazane having this structural formula can react with a hydroxyl group on the reactive silicon group of the silicone-modified polyester resin or a hydroxyl group formed by hydrolysis of a hydrolyzable group on the reactive silicon group to form an Si — O — Si bond having excellent heat resistance, and an imino group in the polysilazane molecule is released as a small molecule of ammonia gas. The reaction principle can be expressed by the following chemical equation:
also present in the amino resin is a high imino resin having the structure:
wherein R represents methyl, n-butyl or isobutyl, and a plurality of R can be the same or different; the alkoxy group of the high imino resin can also be subjected to condensation reaction with the reactive silicon group of the organic silicon modified polyester resin to form a Si-O-C bond with good heat resistance. However, the high imino resin contains many active imino (-NH) in its molecule, and is susceptible to heat or ultraviolet irradiation, resulting in yellowing. Therefore, in the use, the high imino resin is not used as much as possible for the function of the touch panel, and the high imino resin may be considered according to the requirement of the effect after performing modification, replacement, and the like on the imino (-NH), or after a corresponding solution is provided to avoid the above problem.
The silanol condensation catalyst used in the invention can promote the condensation reaction between the hydroxyl bonded with the silicon atom and the alkoxy, acyloxy, ketoximino or alkenyloxy bonded with the silicon atom, and finally the interaction between the components and the main material is combined to improve the property of the ink product. The silanol condensing catalyst used in the present invention is at least one selected from the group consisting of inorganic acids, inorganic bases, organic acids, organic amine compounds and organometallic compounds.
Among them, inorganic acids such as hydrochloric acid, sulfuric acid, nitric acid, etc.; inorganic bases such as sodium hydroxide, potassium hydroxide, and aqueous ammonia; organic acids, mainly organic carboxylic acids with 1-20 carbon atoms, such as oxalic acid, formic acid, acetic acid, propionic acid, octanoic acid, decanoic acid, benzoic acid, and the like; organic amine compounds such as ethylamine, ethylenediamine, n-hexylamine, triethylamine, triethanolamine, pyridine, 1,3, 3-tetramethylguanidinopropyltriethoxysilane, 1,3, 3-tetramethylguanidinopropyltrimethoxysilane, tetramethylammonium hydroxide, tetraethylammonium hydroxide and the like.
Organic metal compounds, from the viewpoint of reducing the functional requirements for dyeing, preferably organic tin compounds, organic titanium compounds, organic zirconium compounds, organic zinc compounds and organic aluminum compounds, organic tin compounds such as dibutyltin dilaurate, dibutyltin diacetate, dibutyltin dioctoate, dibutyltin maleate, dibutyltin dimethylmaleate, dioctyltin diacetate, dioctyltin distearate, dioctyltin dilaurate, stannous octoate, dibutyltin oxide, dioctyltin oxide, di-n-butyl bis (acetylacetonato) tin, tin acetylacetonate; organic titanium compounds such as tetraisopropyl titanate, tetrabutyl titanate, titanium tetrakis (acetylacetonate), titanium diisopropoxybis (ethylacetoacetate), titanium diisopropoxybis (acetoacetate), and titanium diisopropoxybis (acetylacetonate); organozirconium compounds such as zirconium tri-n-butoxide (ethylacetoacetate), zirconium di-n-butoxide (ethylacetoacetate), zirconium tri-n-butoxide (ethylacetoacetate), zirconium tetra (n-propylacetoacetate), zirconium tetra (acetoacetoacetate), zirconium tetra (ethylacetoacetate), zirconium tri-n-butoxide (acetylacetonate), zirconium tetra (acetylacetonate); examples of the organic based zinc compounds include zinc octylate, zinc benzoate, zinc p-tert-butylbenzoate, zinc naphthenate, zinc laurate, zinc stearate, zinc acetylacetonate, and the like; examples of the organic aluminum compound include trimethoxyaluminum, triethoxyaluminum, triisobutoxyaluminum, triisopropoxyaluminum, diisopropoxyaluminum (ethylacetoacetate), diisobutoxyaluminum (ethylacetoacetate), diisopropoxyaluminum (acetoacetate), isopropoxyaluminum (ethylacetoacetate), isopropoxyaluminum (acetylacetonate), tris (ethylacetoacetate), tris (acetylacetonate) aluminum, and monoacetylaluminum bis (ethylacetoacetate).
The amount of the silanol condensing catalyst is controlled to 0.01 to 1 part by weight based on 100 parts by weight of the silicone modified polyester resin. If the silanol condensing catalyst is used in an amount of less than 0.01 parts by weight, the acceleration of the silanol condensation reaction is insignificant. If the silanol condensing catalyst is used in an amount of more than 1 part by weight, the curing reaction is caused too fast, and the viscosity of the ink composition increases too fast during printing, resulting in a decrease in printing quality. Too high a silanol condensation catalyst level may also have the effect of staining the ink, reducing the resistance of the paint film, etc. Of course, 0.05 to 0.5 parts by weight is selected for optimum and stable balance of properties.
The polyorganosiloxane antifoaming agent used in the present invention is at least one selected from the group consisting of alkyl-modified polyorganosiloxane antifoaming agents and fluoroalkyl-modified polyorganosiloxane antifoaming agents. These two classes of antifoam agents have the general formula:
wherein R represents an alkyl group or a fluoroalkyl group. The main chain frameworks of the two types of defoaming agents are Si-O-Si bonds, and the main chain frameworks are similar to the structural mechanism of the main material, so that the excellent high-temperature resistance of the ink is realized through cooperative promotion. The amount ratio is most effective in terms of properties, and the polyorganosiloxane defoamer is used in an amount of 0.1 to 4 parts by weight based on 100 parts by weight of the silicone modified polyester resin.
The alkyl and/or aralkyl modified polyorganosiloxane leveling agent used in the present invention has the following structure:
wherein R represents an alkaneAnd/or aralkyl. The main chain skeleton of the leveling agent is Si-O-Si bond with excellent heat resistance, and the side chain is connected with alkyl or aralkyl, so the leveling agent has good yellowing resistance at high temperature. The alkyl and/or aralkyl modified polyorganosiloxane leveling agent is used in an amount of 0.1 to 4 parts by weight based on 100 parts by weight of the organosilicon modified polyester resin. The polyether modified organic silicon flatting agent and the polyester modified organic silicon flatting agent have structures similar to alkyl and/or aralkyl modified organic siloxane flatting agent. Polyether is used in the polyether modified organosilicon leveling agent to replace the R group position in the structural formula. The polyethers contain chain members of the Epoxyethyl (EO) and/or epoxypropyl (PO) group. The ether bond (C-O-C) is easy to break at high temperature, so that the printing ink composition containing the polyether modified organic silicon leveling agent is easy to yellow at high temperature. The R group position in the structural formula of the polyester modified organic silicon flatting agent is polyester. Polyester modified silicone leveling agents have heat resistance superior to polyether modified silicone leveling agents, but still cannot withstand high temperatures above 250 ℃. Other leveling agents that do not contain silicone, such as polyacrylate leveling agents and fluorocarbon-modified polyacrylate leveling agents, have poor high temperature resistance because the backbone skeleton is a C — C bond. Therefore, the present invention can be adopted to reduce the number of the adopted components as much as possible, and of course, if the above-mentioned drawbacks are solved by the inventive means, the present invention can be adopted according to the effect.
Further, the solvent used in the present invention is mainly used as a dispersion medium of the ink, and is not particularly limited, but ketones, alcohols, esters, ether esters, alcohol ethers, aliphatic hydrocarbons, aromatic hydrocarbon solvents, and mixtures thereof are preferable, and esters, ether esters, alcohol ethers, aromatic hydrocarbon solvents, and mixtures thereof are more preferable. The solvent is used in an amount of 50 to 150 parts by weight based on 100 parts by weight of the silicone-modified polyester resin. For the effect of the overall viscosity and printability of the ink, the solvent is preferably used in an amount such that the solid content of the high temperature resistant white glass ink composition of the present invention is in the range of 60% to 80%. Wherein,
as the ester solvent, there are ethyl acetate, butyl acetate, γ -butyrolactone, methyl lactate, ethyl lactate, dimethyl succinate, dimethyl glutarate, dimethyl adipate, DBE, pentyl valerate, isoamyl acetate, isobutyl acetate, butyl propionate, isopropyl butyrate, ethyl butyrate, butyl butyrate and the like.
Examples of the ether ester solvents include ethylene glycol monomethyl ether acetate, ethylene glycol ethyl ether acetate, ethylene glycol monobutyl ether acetate, propylene glycol monomethyl ether acetate, propylene glycol monoethyl ether acetate, propylene glycol butyl ether acetate, diethylene glycol methyl ether acetate, diethylene glycol ethyl ether acetate, diethylene glycol propyl ether acetate, diethylene glycol isopropyl ether acetate, diethylene glycol butyl ether acetate, diethylene glycol tert-butyl ether acetate, triethylene glycol methyl ether acetate, ethyl 3-methoxypropionate, ethyl 3-ethoxypropionate, and methyl 3-ethoxypropionate.
Examples of the alcohol ether solvents include ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monopropyl ether, ethylene glycol monoisopropyl ether, ethylene glycol monobutyl ether, ethylene glycol monohexyl ether, ethylene glycol dimethyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl ether, propylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol dimethyl ether, and diethylene glycol diethyl ether.
The invention further provides a preparation method of the high-temperature-resistant ink, which comprises the following steps:
before preparation, raw materials can be obtained according to the reference in the ingredient components;
s10, mixing 30-100 parts by weight of organic silicon modified polyester resin, 60-240 parts by weight of rutile titanium dioxide, 0.5-10 parts by weight of fumed silica and a proper amount of solvent, and dispersing at high speed for 10-60 minutes to form dispersed slurry;
s20, grinding and dispersing the dispersed slurry by using a grinder until the fineness reaches below 10 mu m, adding the balance of organic silicon modified polyester resin, a proper amount of solvent, 0.1-4 parts by weight of organic polysiloxane antifoaming agent and 0.1-4 parts by weight of alkyl and/or aralkyl modified organic polysiloxane flatting agent, and uniformly stirring to obtain a main agent of the ink;
s30, uniformly mixing 1-30 parts by weight of cross-linking agent, 0.01-1 part by weight of silanol condensation catalyst and a proper amount of solvent to obtain the curing agent of the ink;
the grinding equipment for grinding treatment in the preparation process can adopt a three-roller machine, a ball mill, a horizontal sand mill, a vertical sand mill, a blue type sand mill and the like. The prepared ink main agent and the curing agent can be stored separately, and in use, the prepared ink main agent and the curing agent are preferably mixed in a ratio of 100:5 or 100:10 from the convenient measurement; after the main agent and the curing agent of the ink are uniformly mixed according to the proportion, the mixture is printed on a glass substrate through a screen printing process, and the glass substrate is baked at 150-200 ℃ for 10-60 minutes to be cured, so that a high-temperature-resistant ink layer can be formed on the surface of the substrate. The screen printing gauze is not particularly limited, and nylon gauze, polyester gauze and stainless steel gauze can be used; for the purpose and effect of precision printing, polyester mesh and stainless steel mesh are preferable, and the mesh number is preferably 350-420 mesh.
To better aid in the understanding of the present invention, and the superior results obtained with the ink products of the present invention, the following examples are given by way of illustration:
example 1
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.5g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(DuPont corporation) and dispersed for 30 minutes at 4000rpm/min using a high speed disperser (with a 3cm diameter dispersion plate) to form a uniformly dispersed slurry;
s20, grinding the dispersed slurry by a three-roll machine until the fineness is below 10 mu m, supplementing 14g of CSH3000 resin, 0.5g of defoaming agent BYK-077(BYK company), 0.5g of flatting agent BYK-322(BYK company) and 3g of DBE solvent, and uniformly stirring to obtain the main agent of the high-temperature resistant white glass ink composition;
s30, 3g of methyltrimethoxysilane, 0.03g of dibutyltin dilaurate Dabco T-12(AIR PRODUCTS) and 2.2g of toluene were mixed uniformly to prepare the curing agent for the high temperature resistant white glass ink composition of the present invention.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test.
Example 2
A high temperature resistant white glass ink composition of the present invention was prepared and tested for performance in the same manner as in example 1 except that the silicone modified polyester resin CSH3000 of example 1 was replaced with a silicone modified polyester resin SRE-906 (having a solid content of 60%, supplied from the Dong-rich chemical raw materials Co., Ltd., Guangzhou city).
Example 3
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.8g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(HUNTSMAN company) and dispersing the mixture for 30 minutes at 4000rpm/min by a high-speed disperser (with a dispersing plate having a diameter of 3 cm) to form a dispersion slurry;
s20, grinding the dispersed slurry by a three-roll machine until the fineness is below 10 mu m, supplementing 14g of CSH3000 resin, 0.5g of defoaming agent BYK-077, 0.5g of flatting agent BYK-322 and 3g of DBE solvent, and uniformly stirring to obtain the main agent of the high-temperature resistant white glass ink composition;
s30, 3g of methyltriacetoxysilane, 0.03g of aluminum tris (acetylacetonate), and 2.21g of toluene were mixed to obtain the curing agent for high temperature resistant white glass ink composition of the present invention.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test.
Example 4
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.8g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(HUNTSMAN company) and dispersing the mixture for 30 minutes at 4000rpm/min by a high-speed disperser (with a dispersing plate having a diameter of 3 cm) to form a dispersion slurry;
s20, then forming a dispersed slurry; grinding the mixture by a three-roller machine until the fineness reaches below 10 mu m, then supplementing 14g of CSH3000 resin, 0.5g of defoaming agent BYK-077, 0.5g of flatting agent BYK-322 and 3g of DBE solvent, and uniformly stirring to obtain the main agent of the high-temperature resistant white glass ink composition;
s30, 4g of methyl tributyl ketoxime silane, 0.06g of aluminum tris (acetylacetonate) and 1.18g of toluene are mixed uniformly to prepare the curing agent of the high-temperature resistant white glass ink composition.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test.
Example 5
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.8g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(HUNTSMAN company) and dispersing the mixture for 30 minutes at 4000rpm/min by a high-speed disperser (with a dispersing plate having a diameter of 3 cm) to form a dispersion slurry;
s20, then forming a dispersed slurry; grinding the mixture by a three-roller machine until the fineness reaches below 10 mu m, then supplementing 14g of CSH3000 resin, 0.5g of defoaming agent BYK-077, 0.5g of flatting agent BYK-322 and 3g of DBE solvent, and uniformly stirring to obtain the main agent of the high-temperature resistant white glass ink composition;
s30, 1.2g of polysilazane DURAZANE1500SC (AZ Electronic Materials Co.) and 0.5g of epoxysilane coupling agent(Evonik Degussa Co., Ltd.), 0.03g of aluminum tris (acetylacetonate) and 3.51g of toluene were mixed uniformly to prepare a curing agent for a high temperature resistant white glass ink composition of the present invention.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test. The test results are reported in table 2.
Example 6
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.8g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(HUNTSMAN company) and dispersing the mixture for 30 minutes at 4000rpm/min by a high-speed disperser (with a dispersing plate having a diameter of 3 cm) to form a dispersion slurry;
s20, grinding the formed dispersed slurry by using a three-roll machine until the fineness reaches below 10 mu m, supplementing 14g of CSH3000 resin, 0.75g of highly n-butyl etherified amino resin CYMEL1156(CYTEC company), 0.5g of defoaming agent BYK-077, 0.5g of flatting agent BYK-322 and 3g of DBE solvent, and uniformly stirring to obtain the main agent of the high-temperature resistant white glass ink composition;
s30, adding 3g of epoxy silane coupling agent(Evonik Degussa Co., Ltd.), 0.06g of aluminum tris (acetylacetonate) and 2.22g of toluene were mixed uniformly to prepare a curing agent for a high temperature resistant white glass ink composition of the present invention.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test.
Example 7
A high temperature resistant white glass ink composition of the present invention was prepared in the same manner as in example 4 except that the defoaming agent BYK-077 in example 4 was replaced with BYK-066N (BYK corporation), and performance tests were performed.
Comparative example 1
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.8g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(HUNTSMAN company) and dispersing the mixture for 30 minutes at 4000rpm/min with a high-speed disperser (having a dispersion disk with a diameter of 3 cm) to form a dispersion slurry;
s20, grinding the formed dispersed slurry by a three-roll machine until the fineness reaches below 10 mu m, supplementing 14g of CSH3000 resin, 0.5g of defoaming agent BYK-077, 0.5g of flatting agent BYK-322 and 3g of DBE solvent, and uniformly stirring to obtain a main agent of the white glass ink composition;
s30, 2.0g of aminosilane coupling agent(Evonik Degussa Co., Ltd.), 0.06g of aluminum tris (acetylacetonate) and 3.18g of toluene were mixed uniformly to prepare a curing agent for a white glass ink composition.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test.
Comparative example 2
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.8g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(HUNTSMAN Co.) mixingDispersing for 30 minutes by a high-speed disperser (with a dispersion disc with the diameter of 3 cm) at the rotating speed of 4000rpm/min to form dispersed slurry;
s20, grinding the formed dispersion slurry by using a three-roll machine until the fineness reaches below 10 mu m, supplementing 14g of CSH3000 resin, 0.75g of high imino resin CYMEL325(CYTEC company), 0.5g of defoaming agent BYK-077, 0.5g of flatting agent BYK-322 and 3g of DBE solvent, and uniformly stirring to obtain a main agent of the white glass ink composition;
s30, 3g of methyltrimethoxysilane, 0.06g of aluminum tris (acetylacetonate), and 2.22g of toluene were mixed uniformly to prepare a curing agent for a white glass ink composition.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test.
Comparative example 3
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.8g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(HUNTSMAN company) and dispersing the mixture for 30 minutes at 4000rpm/min by a high-speed disperser (with a dispersing plate having a diameter of 3 cm) to form a dispersion slurry;
s20, grinding the formed dispersed slurry by a three-roll machine until the fineness reaches below 10 mu m, supplementing 14g of CSH3000 resin, 0.5g of defoaming agent BYK-077, 0.5g of flatting agent BYK-322 and 3g of DBE solvent, and uniformly stirring to obtain a main agent of the white glass ink composition;
s30, 2.0g of blocked polyisocyanate curing agentSN (Bayer Corp.) 0.5g of an epoxysilane coupling agent(Evonik Degussa Co., Ltd.), 0.06g of aluminum tris (acetylacetonate) and 2.68g of toluene were mixed uniformly to prepare a curing agent for a white glass ink composition.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test.
Comparative example 4
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.8g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(HUNTSMAN company) and dispersing the mixture for 30 minutes at 4000rpm/min by a high-speed disperser (with a dispersing plate having a diameter of 3 cm) to form a dispersion slurry;
s20, grinding the formed dispersion slurry by a three-roll machine until the fineness reaches below 10 mu m, supplementing 14g of CSH3000 resin, 0.5g of defoaming agent BYK-077, 0.5g of fluorocarbon modified polyacrylate flatting agent Afcona-3777S (Afcona company) and 3g of DBE solvent, and uniformly stirring to obtain a main agent of the white glass ink composition;
s30, 4g of methyltributanoxime silane, 0.06g of aluminum tris (acetylacetonate), and 1.18g of toluene were mixed uniformly to prepare a curing agent for a white glass ink composition.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test.
Comparative example 5
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.8g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(HUNTSMAN company) and dispersing the mixture for 30 minutes at 4000rpm/min by a high-speed disperser (with a dispersing plate having a diameter of 3 cm) to form a dispersion slurry;
s20, grinding the formed dispersed slurry by a three-roll machine until the fineness reaches below 10 mu m, and supplementing 14g of CSH3000 resin, 0.5g of defoaming agent BYK-077 and 0.5g of polyether polyester copolymerization modified polyorganosiloxane leveling agent(Storocco chemical Co., Ltd., Guangzhou) and 3g of DBE solvent were uniformly stirred to prepare a main agent of a white glass ink composition;
s30, 4g of methyltributanoxime silane, 0.06g of aluminum tris (acetylacetonate), and 1.18g of toluene were mixed uniformly to prepare a curing agent for a white glass ink composition.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test.
Comparative example 6
S10, mixing 36g of organic silicon modified polyester resin CSH3000 (solid content is 60%, provided by Shenzhen Chuangshihengten Co., Ltd.) and 0.8g of fumed silica(Evonik Degussa Co.) and 50g of rutile type titanium dioxide(HUNTSMAN company) and dispersing the mixture for 30 minutes at 4000rpm/min with a high-speed disperser (having a dispersion disk with a diameter of 3 cm) to form a dispersion slurry;
s20, grinding the formed dispersed slurry by a three-roll machine until the fineness is below 10 mu m, supplementing 14g of CSH3000 resin, 0.5g of non-silicon defoamer Afcona-2720(Afcona company), 0.5g of leveling agent BYK-322 and 3g of DBE solvent, and uniformly stirring to obtain the main agent of the white glass ink composition;
s30, 4g of methyltributanoxime silane, 0.06g of aluminum tris (acetylacetonate), and 1.18g of toluene were mixed uniformly to prepare a curing agent for a white glass ink composition.
And (3) uniformly mixing the main agent and the curing agent of the ink according to the proportion of 100:5 to prepare a glass lens sample, and carrying out performance test.
The glass lens samples obtained in the above examples and comparative examples were subjected to performance tests including:
(1) and (3) testing pencil hardness: the pencil hardness of the paint film was tested according to GB/T6739 determination of paint film hardness by 2006 color paint and varnish pencil method.
(2) And (3) testing the adhesive force: the adhesion of the paint films was tested according to the "GB/T9286-1998 cut and rule test for paint and varnish films".
(3) Boiling water resistance test: and (3) placing the glass lens sample in a boiling test box, boiling the glass lens sample in deionized water at 100 ℃ for 1 hour under normal pressure, taking out the glass lens sample, airing the glass lens sample for 24 hours, observing the appearance change of a paint film, and testing the adhesive force of the paint film.
(4) Butanone resistance test: dipping white soft dustless cloth in chemical pure butanone, applying 500g of force, wiping the paint film back and forth for 50 times, and observing whether the dustless cloth is dyed or not, and whether the paint film is damaged, falls off or fades.
(5) Testing inorganic developing solution resistance: and soaking the glass lens sample in an inorganic developing solution for 1000 seconds, taking out and airing for 24 hours, observing the appearance change of the paint film, and testing the adhesive force of the paint film.
(6) And (3) testing the photoresist stripping liquid resistance: and soaking the glass lens sample in the photoresist stripping liquid for 1000 seconds, taking out and airing for 24 hours, observing the appearance change of the paint film, and testing the adhesive force of the paint film.
(7) Testing of ITO (indium tin oxide) etching solution: and soaking the glass lens sample in the ITO etching solution for 1000 seconds, taking out and airing for 24 hours, observing the appearance change of the paint film, and testing the adhesive force of the paint film.
(8) And (3) high temperature resistance test: and (3) putting the glass lens sample into a blast drying oven at 300 ℃ for baking for 30min, taking out the glass lens sample, naturally cooling for 2 hours, observing the appearance change of a paint film, and testing the adhesive force of the paint film.
(8) High temperature and high humidity resistance test: and (3) placing the glass lens sample in a test environment with the temperature of 60 ℃ and the humidity of 95% RH for storage for 120 hours, taking out and airing for 24 hours, observing the appearance change of the paint film, and testing the adhesive force of the paint film.
(9) And (3) high and low temperature impact resistance test: the glass lens samples were placed in a cold-hot impact test chamber for a cold-hot impact test as in table 1 below, repeated for 40 cycles, taken out and observed for changes in the appearance of the paint film, and the adhesion of the paint film was tested.
| Temperature of | 80℃ | At room temperature | -20℃ | At room temperature |
| Time of day | 2 hours | 0.5 hour | 2 hours | 0.5 hour |
(10) Salt spray resistance test: referring to GB/T1771-2007 color paint and varnish neutral salt spray resistance performance determination, a glass lens sample is subjected to a neutral salt spray experiment for 120 hours, the glass lens sample is taken out and aired for 24 hours, then the appearance change of a paint film is observed, and the adhesion of the paint film is tested.
The test results are given in table 2 below:
as can be seen from table 2, the high temperature resistant white glass ink composition of the present invention has excellent adhesion to glass substrates and good chemical resistance, and more importantly, has significantly improved high temperature yellowing resistance. Comparative example 1 used an aminosilane coupling agent, and comparative examples 2 and 3 used a high imino resin CYMEL325 and a blocked polyisocyanate curing agent, respectivelySN As a crosslinking agent, in comparative example 4, Afcona-3777s, which is a fluorocarbon-modified polyacrylate leveling agent, and in comparative example 5, a polyether-polyester copolymer-modified polyorganosiloxane leveling agentComparative example 6, in which a non-silicon defoaming agent Afcona-2720 was used, resulted in significant deterioration in yellowing resistance of the white ink composition at high temperatures. And aspects of the ink products produced in the present inventionCompared with the prior ink, the performance of (1), especially the heat resistance and the yellowing resistance, is obviously improved.
The invention further provides an OGS touch panel prepared by using the high-temperature resistant ink. By adopting the high-temperature-resistant ink, the ink main agent and the curing agent are prepared step by step, and are finally mixed and cured, then the high-temperature-resistant ink prepared in the invention is used in an OGS (one glass solution) process, and finally the OGS touch panel prepared by adopting the high-temperature-resistant ink is obtained; the process is simple, and the stable property and the optimal effect of the ink can be guaranteed to the maximum extent. The OGS touch panel prepared by the high-temperature-resistant ink has the advantages that the ink property is not changed and is not yellowed after subsequent processes such as high temperature, film coating, etching and the like; the display effect is better.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The high-temperature-resistant ink is characterized by comprising the following components in parts by mass:
100 parts of organic silicon modified resin, 60-240 parts of titanium dioxide, 0.5-10 parts of fumed silica, 1-30 parts of a cross-linking agent, 0.01-1 part of silanol condensation catalyst, 0.1-4 parts of a polysiloxane defoaming agent, 0.1-4 parts of an alkyl and/or aralkyl modified polysiloxane flatting agent and 50-150 parts of a solvent.
2. The high temperature resistant ink of claim 1,the organic silicon modified resin is characterized in that molecules of the organic silicon modified resin contain at least 1 reactive silicon group, and the reactive silicon group comprises the following groups:wherein,
in the formula R1And R2Is alkyl with 1-20 carbon atoms, aryl with 6-20 carbon atoms or aralkyl with 7-20 carbon atoms; x is hydroxyl or a hydrolyzable group; m is an integer of 1 to 3, and n is an integer of 1 to 2.
3. The high temperature resistant ink according to claim 1 or 2, wherein the crosslinking agent is at least one of a silane crosslinking agent, an epoxy silane coupling agent, an amino resin, and a polysilazane.
4. The high temperature resistant ink of claim 3, wherein the silane crosslinking agent comprises the structure: rnSiX4-nN is an integer of 0 to 2; wherein R is selected from alkyl with 1-10 carbon atoms, aryl with 6-10 carbon atoms or aralkyl with 7-10 carbon atoms; x is at least one of alkoxy, acyloxy, ketoximino and alkenyloxy.
5. The high temperature ink of claim 3, wherein the epoxysilane coupling agent is one or more of gamma- (2, 3-epoxypropoxy) propyltrimethoxysilane, gamma- (2, 3-epoxypropoxy) propyltriethoxysilane, gamma- (2, 3-epoxypropoxy) propylmethyldimethoxysilane, and gamma- (2, 3-epoxypropoxy) propylmethyldiethoxysilane.
6. The high temperature resistant ink according to claim 3, wherein the amino resin is one or a mixture of highly methylated amino resin, highly butylated amino resin, highly etherified phenylated amino resin and highly etherified mixedly etherified amino resin.
7. The high temperature resistant ink of claim 1 or 2, wherein the polyorganosiloxane defoamer is at least one of an alkyl-modified polyorganosiloxane defoamer and a fluoroalkyl-modified polyorganosiloxane defoamer;
and/or the presence of a catalyst in the reaction mixture,
the silanol condensation catalyst is at least one of inorganic acid, inorganic base, organic acid, organic amine compound and organic metal compound;
and/or the presence of a catalyst in the reaction mixture,
the titanium dioxide is rutile type titanium dioxide with the particle size of 0.15-0.50 mu m.
8. The method for preparing a high temperature resistant ink according to any one of claims 1 to 7, comprising the steps of:
mixing 30-100 parts by weight of raw materials in 100 parts by weight of organic silicon modified polyester resin with rutile titanium dioxide and a part of solvent for fumed silica, and uniformly dispersing to form dispersed slurry;
grinding and dispersing the dispersed slurry until the fineness is below 10 mu m, adding the rest organic silicon modified polyester resin, the organic polysiloxane defoaming agent, the alkyl and/or aralkyl modified organic polysiloxane flatting agent and part of solvent, and uniformly mixing to obtain the main printing ink agent;
and uniformly mixing the cross-linking agent, the silanol condensation catalyst and the residual solvent to obtain the ink curing agent.
9. The method for preparing a high temperature resistant ink according to claim 8, wherein the step of uniformly mixing the cross-linking agent, the silanol condensing catalyst and the remaining solvent to obtain the ink curing agent further comprises the steps of:
and (3) uniformly mixing the ink main agent and the ink curing agent, printing the mixture on a base material through screen printing, and then carrying out curing treatment.
10. An OGS touch panel comprising the high temperature resistant ink of any one of claims 1 to 7.
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