CN104497944B - One can develop UV solidify hydrofluoric acid resistant protection glue - Google Patents
One can develop UV solidify hydrofluoric acid resistant protection glue Download PDFInfo
- Publication number
- CN104497944B CN104497944B CN201410660397.7A CN201410660397A CN104497944B CN 104497944 B CN104497944 B CN 104497944B CN 201410660397 A CN201410660397 A CN 201410660397A CN 104497944 B CN104497944 B CN 104497944B
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- Prior art keywords
- acrylate
- pigment yellow
- hydrofluoric acid
- acid resistant
- develop
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- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 239000003292 glue Substances 0.000 title claims abstract description 44
- 229920005989 resin Polymers 0.000 claims abstract description 48
- 239000011347 resin Substances 0.000 claims abstract description 48
- 239000000178 monomer Substances 0.000 claims abstract description 33
- 239000011159 matrix material Substances 0.000 claims abstract description 14
- -1 anhydride modified epoxy acrylate Chemical class 0.000 claims description 44
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 40
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical group COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 36
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 33
- 239000000203 mixture Substances 0.000 claims description 27
- 239000004593 Epoxy Substances 0.000 claims description 24
- 229910052731 fluorine Inorganic materials 0.000 claims description 20
- 239000011737 fluorine Substances 0.000 claims description 17
- 239000002253 acid Substances 0.000 claims description 16
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 15
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 14
- 239000012752 auxiliary agent Substances 0.000 claims description 14
- 239000000945 filler Substances 0.000 claims description 14
- 239000004925 Acrylic resin Substances 0.000 claims description 13
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 12
- 239000004814 polyurethane Substances 0.000 claims description 12
- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 claims description 12
- YJKHMSPWWGBKTN-UHFFFAOYSA-N 2,2,3,3,4,4,5,5,6,6,7,7-dodecafluoroheptyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)F YJKHMSPWWGBKTN-UHFFFAOYSA-N 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 11
- UHESRSKEBRADOO-UHFFFAOYSA-N ethyl carbamate;prop-2-enoic acid Chemical compound OC(=O)C=C.CCOC(N)=O UHESRSKEBRADOO-UHFFFAOYSA-N 0.000 claims description 10
- DEQJNIVTRAWAMD-UHFFFAOYSA-N 1,1,2,4,4,4-hexafluorobutyl prop-2-enoate Chemical compound FC(F)(F)CC(F)C(F)(F)OC(=O)C=C DEQJNIVTRAWAMD-UHFFFAOYSA-N 0.000 claims description 9
- 244000284380 Hibiscus rosa sinensis Species 0.000 claims description 9
- 235000000664 Rosa chinensis Nutrition 0.000 claims description 9
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- 238000006243 chemical reaction Methods 0.000 claims description 8
- 150000001875 compounds Chemical class 0.000 claims description 8
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- QTKPMCIBUROOGY-UHFFFAOYSA-N 2,2,2-trifluoroethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)F QTKPMCIBUROOGY-UHFFFAOYSA-N 0.000 claims description 3
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 3
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- 241001597008 Nomeidae Species 0.000 claims description 2
- 150000001252 acrylic acid derivatives Chemical class 0.000 claims description 2
- WURBFLDFSFBTLW-UHFFFAOYSA-N benzil Chemical compound C=1C=CC=CC=1C(=O)C(=O)C1=CC=CC=C1 WURBFLDFSFBTLW-UHFFFAOYSA-N 0.000 claims description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
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- 238000000034 method Methods 0.000 description 19
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- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 11
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- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 9
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 8
- 239000012467 final product Substances 0.000 description 8
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- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 description 6
- 239000012528 membrane Substances 0.000 description 6
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- 239000007921 spray Substances 0.000 description 4
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Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses the one UV that can develop and solidify hydrofluoric acid resistant protection glue, by mass percentage, it mainly comprises as matrix resin 15～75%, assisted resin 10～55%, activated monomer 6～30%.This UV that can develop solidifies hydrofluoric acid resistant protection glue, has the stickiness protecting glue more excellent than the hydrofluoric acid resistant of prior art, glass especially has high adhesive strength, and hydrofluoric acid resistant etching performance is excellent.
Description
Technical field
The present invention relates to the one UV that can develop and solidify hydrofluoric acid resistant protection glue, be specifically related to one and be applied to etch smooth and groove that desiccant can be held the developed UV in bottom on display of organic electroluminescence (OLED) glass cover-plate and solidify hydrofluoric acid resistant protection glue.
Background technology
OLED, i.e. Organic Light Emitting Diode (OrganicLightEmittingDiode), it is also called Organic Electricity laser display (OrganicElectroLuminescenceDisplay, OELD), it is flat-panel screens technology of new generation after TFT-LCD (ThinFilmTransistorLiquidCrystalDisplay).OLED is different from traditional LCD display mode, belongs to self-luminescent material, it is not necessary to backlight, adopts very thin coating of organic material and glass substrate, and when there being electric current to pass through, these organic materials will be luminous.Additionally, OLED possesses simple structure, contrast height, thickness is thin, visual angle is wide, image quality is uniform, response speed is fast, be easier to colorization, can reach luminescence by simple drive circuit, processing procedure is simple, can be fabricated to flexure formula panel, meeting compact principle, range of application belongs to small-medium size panel.
In display of organic electroluminescence, the existing luminous organic material life-span on average all can reach 15, more than 000 hour, can apply on the volume production commodity of reality, but luminous organic material has a shortcoming: meet water and chance oxygen easily lost efficacy, if can fully prevent pollution and the erosion of aqueous vapor in OLED encapsulation process, then the life-span of element is likely to be lifted up again.
In the production process of OLED, in order to prevent luminous organic material from meeting water and meeting oxygen and easily lost efficacy, it is generally adopted the glass substrate before it and adds back shroud and be packaged, in order to isolation steam and oxygen, the service life of prolonged display.Cover plate conventional in current OLED encapsulation process is: metal cover board, glass cover-plate or thin film are packaged.Wherein metal cover board is different from the coefficient of expansion of glass, it is easy to make device deform, and cost is high, and metal cover board is eliminated gradually；And thin film encapsulation technology is ripe not enough, being limited by the restriction of material, distance volume production is practical also has certain distance, generally all selects glass cover-plate in current industry.OLED process requirements etches the groove that a range of bottom is smooth on glass cover-plate, loads desiccant in groove, also has simultaneously and etches high-precision register guide, in order to para-position laminating accurate with the base plate glass of display.
The manufacture method of glass cover-plate is: be first coated with thicker anti-etching protecting film in the front and rear surfaces of plate glass; then the mode exposed in the wherein one side of glass produces groove pattern; protecting film in developed removal pattern; it is placed in etch liquids and etches groove, finally remove the protecting film of glass surface.
The hydrofluoric acid resistant protection glue of prior art is that protecting film is not enough with the adhesion of glass surface on the one hand, it is easy to comes off, causes a large amount of defect, increases cost；After on the other hand protecting film solidifies, compactness is not enough, cause acid solution can osmotic protection film thus etching glass substrate.
Summary of the invention
The technical problem to be solved is: providing one can meet OLED encapsulation precision requirement, high efficiency, cost are low, has again high adhesion force, and excellent acid-proof alkaline and production is the developed UV solidification hydrofluoric acid resistant protection glue of the easily demoulding again after completing.
For solving above-mentioned technical problem, the technical solution adopted in the present invention is: one can develop UV solidify hydrofluoric acid resistant protection glue, by mass percentage, its composition includes: matrix resin 15～75%, assisted resin 10～55%, activated monomer 6～30%.
Described matrix resin is one or both the mixture in bisphenol A epoxy acrylate, epoxy soybean oil acrylate, PU modified epoxy acrylate resin, anhydride modified epoxy acrylate, Chinese rose acid modified epoxy acrylic ester；One or both mixture in polyether based polyurethanes acrylate, epoxy acrylate, urethane acrylate, PBAA ester；Matrix resin provides the fundamental property of curable adhesive, should have suitable caking property, hydrofluoric acid resistance and stability, therefore the present invention has selected bisphenol A epoxy acrylate, epoxy soybean oil acrylate, PU modified epoxy acrylate resin, anhydride modified epoxy acrylate or Chinese rose acid modified epoxy acrylic ester as matrix resin, this kind of except the feature having epoxy bond function admirable, also have both unsaturated polyester resin fast to solidify, operate adjustable characteristic, be provided simultaneously with the chemical resistance of excellence, solvent resistance and deep drawing quality.Bisphenol A epoxy acrylate is the vinylite by being synthesized by methacrylic acid and bisphenol A epoxide resin, the type resin double bond at strand two ends is extremely active, make vinylite energy rapid solidification, quickly obtain working strength, obtain that there is high corrosion resistance polymer；Further, since adopt methacrylic acid synthesis, the methyl on ester bond limit can shield, and improves hydrolytic resistance；Owing in resin, the amount containing ester bond is few so that it is alkaline resistance properties improves；More secondary hydroxyl can improve the wettability to glass fibre and caking property so that it is mechanical strength improves.Epoxy soybean oil acrylate is the vinylite being synthesized by the epoxy bond in epoxy resin and acrylic acid carboxyl esterification, the double bond at strand two ends makes its curing rate fast, obtain that there is high corrosion resistance polymer, additionally, such resin viscosity is low, zest is little, and pigment has the wettability of excellence.PU modified epoxy vinyl ester resin, compared with other vinyl ester resin, has the corrosion resistance of excellence, pliability and good process, due to the introducing of carbamate, improves the compatibility of resin and fiber, and can keep the air-drying property that resin surface is good.Maleic anhydride modified epoxy acrylate and Chinese rose acid modified epoxy acrylic ester have that curing rate is fast, case hardness is high, substrate wetting good, be effectively improved coating and base material adhesive force, wherein due to the introducing of maleic anhydride, improve the performances such as the unconcerned adhesive force of the painting after heat cure, resistance to acids and bases and solvent resistance, and the introducing of the Chinese rose acid of Long carbon chain, enhance the wettability of resin and pigment on the one hand, resistance to acids and bases, improves the hydrolytic resistance of resin on the other hand.
Described assisted resin is one or both the mixture in aliphatic urethane acrylate, amino acrylic resin, PBAA ester, polyester acrylate.Assisted resin is to add to adjust the bulk property of adhesive, compensate for some of matrix resin not enough, for instance hot strength, high temperature resistant character, hardness etc..Polyether based polyurethanes acrylate is through base Lipase absobed by polyether polyhydroxy-compound, isocyanates and acrylic acid.Polyether polyhydroxy-compound uses conventional PTMEG, for instance Polyethylene Glycol, polypropylene glycol etc.；Isocyanates uses 2,4 toluene diisocyanate or isofoer diisocyanate；Crylic acid hydroxy ester is 2-(Acryloyloxy)ethanol (HEMA) and acrylic acid (HPMA)；Urethane acrylate can increase the compliance of solidification figure layer, reduction stress shrinks, improves adhesive force；PBAA ester has good moisture-proof effect, also has good resistance to low temperature simultaneously.
Described developed UV solidifies in hydrofluoric acid resistant protection glue component, it is preferable that the polyesters compound containing 2～6 acrylate-functional groups.
The preferred degree of functionality of described matrix resin be 2 and viscosity be 5500～45, the resin of 000mPa.s (25 DEG C) or combination, the preferred degree of functionality of assisted resin be 2～6 and viscosity be 1500～10, the resin of 000mPa.s (25 DEG C) or its combination.The modest viscosity of these resins, solidification process shrinkage factor is relatively low, has good film forming and adhesion property.The commercial prod of these resins has the CN111 of Sartomer Company, CN117, CN118, CN119, CN120, CN151, CN962, CN966J75, CN985B88, CN2279, CN2900, CN3001 etc., the 6131-1 of Changxing chemical company, 611A-85, 6134A-80, 615-100, 6141H-80, 6141-100, 6314C-60L etc., the R-115 of Nippon chemical company, R-130, ZAR-1035, ZFR-1122, ZFR-1401H etc., the EpoxyEster40EM of Kyoeisha chemical company, EpoxyEster70PA, EpoxyEster200PA, EpoxyEster80MFA, EpoxyEster3002M, EpoxyEster3002A, EpoxyEster3000M etc., the Photomer6230 etc. of Cognis company.
Described resin more preferably CN111, CN966J75, CN985B88 and/or 61131-1,6141H-80,6314C-60L and/or EpoxyEster3002M, poxyEster3000M.
One or more in simple function group, difunctional or multi-functional acrylate containing fluorine activated monomer of described activated monomer, one or more in simple function group, difunctional or multi-functional vinyl compound activated monomer.The effect of described activated monomer is regulation system viscosity, the wettability promoting adhesive and glass, improves curing rate and improve the various performances of material before and after solidification, such as pliability, hardness, hydrolytic resistance, corrosion resistance etc..The resin that acrylate containing fluorine monomer UV is formed after solidifying has " three high ", " two hate ", i.e. high surface, high heat-resistant stability and high chemical stability；Its fluorine-containing alkyl not only hydrophobic but also hate oil；Monofunctional monomers containing functional group can improve adhesive property in UV solidifies, and polyfunctional monomer can improve resin decay resistance after solidification by improving crosslink density.
One or more in following substances of described acrylate containing fluorine activated monomer: fluorinated acrylate selects hexafluorobutyl acrylate, Hexafluorobutyl mathacrylate, trifluoroethyl methacrylate, dodecafluoroheptyl methacrylate, dodecafluorhe-ptylacrylate, acrylic acid 19 fluorine ester.Acrylate containing fluorine activated monomer has high surface, and the special nature of high heat-resistant stability and high chemical stability is by the structures shape of fluorine atom.F element is the element that electronegativity is maximum, and the hydrogen atom in carbochain is replaced by fluorine atoms rear bond energy increases 72KJ/mol, therefore heat stability is high；Fluorine atom volume is big compared with hydrogen atom, but being derived from less than other any elements, C-C key is protected because of the shielding action of fluorine atom, even if minimum atom is also difficult to wedge, therefore fluorine surfactant has higher heat-resisting and chemical stability；More weak compared with hydrocarbon chain of the interaction force of fluorocarbon chain, therefore it has higher hydro-oleophobicity.Acrylate containing fluorine resin will not react with various strong oxidizers, highly basic and strong acid and decompose, and remains to keep good surface activity in this solution.
Described acrylate containing fluorine activated monomer is it is preferred that from hexafluorobutyl acrylate, Hexafluorobutyl mathacrylate, trifluoroethyl methacrylate, dodecafluoroheptyl methacrylate, dodecafluorhe-ptylacrylate, one or more in acrylic acid 19 fluorine ester.
Described vinyl compound activated monomer comprises at least one ethylene unsaturated bond.The ethylene unsaturated bond of olefinically unsaturated compounds with the radical reaction produced by Photoepolymerizationinitiater initiater in case cause be polymerized, make olefinically unsaturated compounds photopolymerization, one or more in following substances of described vinyl compound activated monomer: ethylene nitrile, styrene, propenyl, (methyl) phenoxy ethyl acrylate, (methyl) ethioxy ethoxyethyl group ester, NVP etc.；Di-functional reactive's monomer such as (methyl) acrylic acid ethylene glycol bisthioglycolate (methyl) acrylate, butanediol two (methyl) acrylate, hexanediol two (methyl) acrylate, tetraethylene-glycol two (methyl) acrylate, dicyclopentadiene acrylate, tripropylene glycol two (methyl) acrylate, Polyethylene Glycol (200) two (methyl) acrylate, Polyethylene Glycol (400) two (methyl) acrylate, Polyethylene Glycol (600) two (methyl) acrylate, Polyethylene Glycol (800) two (methyl) acrylate, trimethylolpropane allyl ether, ethylene glycol (methyl) acrylate, diethylene glycol two (methyl) acrylate, propylene glycol two (methyl) acrylate, trimethylolpropane two (methyl) acrylate, ethylene glycol crotonates, diethylene glycol two crotonates, propylene glycol two crotonates, trimethylolpropane two crotonates, EGMa, diethylene glycol dimaleate, propylene glycol dimaleate, trimethylolpropane dimaleate etc.；Polyfunctional group activated monomer such as trimethylolpropane tris (methyl) acrylate, ethoxylated trimethylolpropane three (methyl) acrylate, trimethylolpropane trimethacrylate, propoxylation trimethylolpropane tris (methyl) acrylate, tetramethylolmethane three (methyl) acrylate, pentaerythritol triallyl ether, two season penta 6 alcohol five (methyl) acrylate, three (methyl) acrylate of trimethylolpropane ethyleneoxide addition, glycerol two (methyl) acrylate, glycerol three (methyl) acrylate, three (methyl) acrylate of glycerol propane ethyleneoxide addition, tetramethylolmethane two (methyl) acrylate, tetramethylolmethane three (methyl) acrylate, tetramethylolmethane four (methyl) acrylate, dipentaerythritol five (methyl) acrylate, dipentaerythritol six (methyl) acrylate, bisphenol-A two (methyl) acrylate, bisphenol-A pair [oxygen ethylene (methyl) acrylate ", bisphenol-A double, two [glycidyl ether (methyl) acrylate], trimethylolpropane tris crotonates, three crotonatess of trimethylolpropane ethyleneoxide addition, glycerol two crotonates, glycerol three crotonates, three crotonatess of glycerol propane ethyleneoxide addition, tetramethylolmethane two crotonates, tetramethylolmethane three crotonates, tetramethylolmethane four crotonates, dipentaerythritol five crotonates, dipentaerythritol six crotonates, bisphenol-A two crotonates, bisphenol-A pair (oxygen ethylene crotonates], double, two [the glycidyl ether crotonates of bisphenol-A, trimethylolpropane tris maleate, three maleates of trimethylolpropane ethyleneoxide addition, glycerol dimaleate, glycerol three maleate, three maleates of glycerol propane ethyleneoxide addition, tetramethylolmethane dimaleate, tetramethylolmethane three maleate, tetramethylolmethane four maleate, dipentaerythritol five maleate, dipentaerythritol six maleate, bisphenol-A dimaleate, bisphenol-A double, two [oxygen EMA ester], bisphenol-A double, two [glycidyl ether maleate] etc.；And the CD9050 (monofunctional acrylate) etc. of the Photomer4039 of some commercial specific functional groups acrylate such as Cognis companies (phenolic group ethyoxyl 3EO mono acrylic ester), Sartomer Company.
Described fluorine-containing activated monomer most preferably hexafluorobutyl acrylate, dodecafluoroheptyl methacrylate, dodecafluorhe-ptylacrylate；Described vinyl compound activated monomer most preferably ethoxylated trimethylolpropane three (methyl) acrylate and/or propoxylation trimethylolpropane tris (methyl) acrylate, tetramethylolmethane three (methyl) acrylate or tetramethylolmethane three maleate.
Described activated monomer is simple function group, difunctional or multi-functional acrylate containing fluorine activated monomer is the mixture of 1:1～1:5 in mass ratio with simple function group, difunctional or multi-functional vinyl compound activated monomer；It is preferably 1:3.
Described developed UV solidifies hydrofluoric acid resistant protection glue, and by mass percentage, it consists of: matrix resin 25～55%; assisted resin 15～35%, activated monomer 8～16%, filler 0.5～20%; light trigger 1～10%, auxiliary agent 0.2～5%, organic pigment 0.1～1%.
Described filler is nano-TiO2, resin adds nano-TiO2Particle, it is possible to improve its corrosion resistance, ageing resistace, improve the wearability of material.
Described light trigger eliminates one or more the mixture in reaction mechanism light trigger, visible light initiator, radical photoinitiator selected from cracking reaction photoinitiator, hydrogen.
Described cracking reaction photoinitiator is benzoin ether, benzil ketals, 1-Phenylethanone., acyl group phosphorous oxide light trigger；It is benzophenone and tertiary amine coordination compound, thioxanthone and derivant, double; two imidazoles that described hydrogen eliminates reaction mechanism light trigger；Described visible light initiator is camphorquinone；Described radical photoinitiator is: Benzoinum contracting methyl ether (CIBA-GEIGY company trade name Irgacure651), 1-hydroxycyclohexyl phenyl ketone (trade name Irgacure184), 2-hydroxy-2-methyl-1-phenyl-1-acetone (trade name Darocure1173), 2-methyl isophthalic acid-(4-methyl mercapto phenyl)-2-morpholine-1-acetone (trade name Irgacure907), 2, 4, 6-trimethylbenzoy-dipheny phosphine oxide (trade name TPO), 2-phenyl benzyl-2-dimethyl amine-1-(4-morpholine benzyl phenyl) butanone (trade name Irgacure369).Preferred Irgacure369, Irgacure907 and/or TPO.Light trigger may be used alone, can also be used in combination, and mainly curing rate as requested, bondline thickness determine.
Described auxiliary agent is adhesion promoter, levelling agent, defoamer, stabilizer, and its mass ratio is 1:1:1:1.Wherein adhesion promoter is selected from the acrylic acid one or more mixture in base Arrcostab, acrylic acid, the acrylate containing Suo Ji functional group or the phosphate ester adhesion promoter containing unsaturated functional group, is one or both in modest 1121 adhesion promoters of moral, SartomerCD9051, the A-172 silane coupler of union carbide corporation, methacrylic acid phosphoric acid ester；Preferred moral modest 1121 or A-172.Antioxidant is one or more of hindered phenol compound, phosphite ester compound, thio-based compound and complex class compound, it is preferable that hindered phenol compound, such as products such as BHT, 2246,1010,1076.Stabilizer is one or more in ferrocene compounds, anhydrides compound, phenol compound, and ferrocene compounds is ferrocene, methyl ferrocene, ethyl dicyclopentadienyl iron；Anhydrides compound is phthalic anhydride, maleic anhydride, succinic anhydrides；Phenol compound is hydroquinone, p methoxy phenol, 2,6 ditertiary butyl p cresol.Preferred ferrocene, methyl ferrocene, ethyl dicyclopentadienyl iron, phthalic anhydride, hydroquinone and/or p methoxy phenol；The solvent-borne type defoamer 2700 or 3100 of defoamer Shi Deqian company, deaeration agent Airex900 or Airex920 etc. of Di Gao company.Preferred solvent type defoamer 3100.
Described organic pigment is arbitrary of the same colour in red, green, blue.
Described red pigment is pyrene series pigments, anthraquione pigmentss are independent or the mixture of a kind of at least within pigment and bisazo system yellow pigment or phosphorus system of India yellow pigment, such as can be selected for the red pigment of following trade name: paratonere 7, paratonere 14, pigment red 41, pigment red 4 8:1, pigment red 4 8:2, pigment red 4 8:3, pigment red 4 8:4, pigment red 146, paratonere 177, paratonere 178, paratonere 184, paratonere 185, paratonere 187, paratonere 200, paratonere 202, paratonere 208, pigment red 21 0, paratonere 246, paratonere 254, paratonere 255, paratonere 264, paratonere 272 etc..Such as can select the yellow uitramarine of following trade name: pigment yellow 1, pigment yellow 2, pigment yellow 3, pigment yellow 4, pigment yellow 5, pigment yellow 6, pigment yellow 10, pigment Yellow 12, pigment yellow 13, pigment Yellow 14, pigment yellow 15, pigment yellow 16, pigment yellow 17, pigment yellow 18, pigment yellow 24, pigment yellow 31, pigment yellow 32, pigment yellow 34, pigment yellow 35, pigment yellow 35:1, pigment yellow 36, pigment yellow 36:1, pigment yellow 37, pigment yellow 37:1, pigment yellow 40, pigment yellow 42, pigment yellow 43, pigment yellow 53, pigment yellow 55, pigment yellow 60, C.I. pigment yellow 61, pigment yellow 62, pigment yellow 63, pigment yellow 65, pigment yellow 73, pigment yellow 74, pigment yellow 77, pigment yellow 81, pigment yellow 83, pigment yellow 93, pigment yellow 94, pigment yellow 95, pigment yellow 97, pigment yellow 98, pigment yellow 100, pigment yellow 101, pigment yellow 104, pigment yellow 106, pigment yellow 108, pigment yellow 109, pigment yellow 110, pigment yellow 113, pigment yellow 114, pigment yellow 115, pigment yellow 116, pigment yellow 117, pigment yellow 118, pigment yellow 119, pigment Yellow 12 0, pigment Yellow 12 6, pigment Yellow 12 7, pigment Yellow 12 8, pigment Yellow 12 9, pigment yellow 13 8, pigment yellow 13 9, pigment yellow 150, pigment yellow 151, pigment yellow 152, pigment yellow 153, pigment yellow 154, pigment yellow 155, pigment yellow 156, pigment yellow 161, pigment yellow 162, pigment yellow 164, pigment yellow 166, pigment yellow 167, pigment yellow 168, pigment yellow 169, pigment yellow 17 0, pigment yellow 17 1, pigment yellow 17 2, pigment yellow 17 3, pigment yellow 17 4, pigment yellow 17 5, pigment yellow 17 6, pigment yellow 17 7, pigment yellow 17 9, pigment yellow 180, pigment yellow 181, pigment yellow 182, pigment yellow 185, pigment yellow 187, pigment yellow 191:1, pigment yellow 199 etc..
Described viridine green be halogenated phthalocyanines series pigments individually or the mixture of its pigment and bisazo system yellow pigment or phosphorus system of India yellow pigment, phthualocyanine pigment is pigment green 36 such as, yellow uitramarine can be azo type pigment, azo condensed type pigment or heterocyclic pigment, or its combination.Such as can select the yellow uitramarine of following trade name: pigment yellow 1, pigment yellow 2, pigment yellow 3, pigment yellow 4, pigment yellow 5, pigment yellow 6, pigment yellow 10, pigment Yellow 12, pigment yellow 13, pigment Yellow 14, pigment yellow 15, pigment yellow 16, pigment yellow 17, pigment yellow 18, pigment yellow 24, pigment yellow 31, pigment yellow 32, pigment yellow 34, pigment yellow 35, pigment yellow 35:1, pigment yellow 36, pigment yellow 36:1, pigment yellow 37, pigment yellow 37:1, pigment yellow 40, pigment yellow 42, pigment yellow 43, pigment yellow 53, pigment yellow 55, pigment yellow 60, C.I. pigment yellow 61, pigment yellow 62, pigment yellow 63, pigment yellow 65, pigment yellow 73, pigment yellow 74, pigment yellow 77, pigment yellow 81, pigment yellow 83, pigment yellow 93, pigment yellow 94, pigment yellow 95, pigment yellow 97, pigment yellow 98, pigment yellow 100, pigment yellow 101, pigment yellow 104, pigment yellow 106, pigment yellow 108, pigment yellow 109, pigment yellow 110, pigment yellow 113, pigment yellow 114, pigment yellow 115, pigment yellow 116, pigment yellow 117, pigment yellow 118, pigment yellow 119, pigment Yellow 12 0, pigment Yellow 12 6, pigment Yellow 12 7, pigment Yellow 12 8, pigment Yellow 12 9, pigment yellow 13 8, pigment yellow 13 9, pigment yellow 150, pigment yellow 151, pigment yellow 152, pigment yellow 153, pigment yellow 154, pigment yellow 155, pigment yellow 156, pigment yellow 161, pigment yellow 162, pigment yellow 164, pigment yellow 166, pigment yellow 167, pigment yellow 168, pigment yellow 169, pigment yellow 17 0, pigment yellow 17 1, pigment yellow 17 2, pigment yellow 17 3, pigment yellow 17 4, pigment yellow 17 5, pigment yellow 17 6, pigment yellow 17 7, pigment yellow 17 9, pigment yellow 180, pigment yellow 181, pigment yellow 182, pigment yellow 185, pigment yellow 187, pigment yellow 191:1, pigment yellow 199 etc., or the mixture of one or more pigment can be used.
Described blue pigment be halogenated phthalocyanines series pigments individually or the mixture of this pigment and dioxazines violet pigment, such as can select the blue pigment of following trade name: pigment blue 15: 1, pigment blue 15: 2, pigment blue 15: 3, pigment blue 15: 3, pigment blue 15: 4, pigment blue 15: 6, pigment blue 16, pigment blue 17, alizarol saphirol 21, alizarol saphirol 22, alizarol saphirol, alizarol saphirol 64, alizarol saphirol 76 etc., violet pigment such as pigment violet 19, pigment Violet 23.
Described developed UV solidifies the compound method of hydrofluoric acid resistant protection glue: add matrix resin and stabilizer in a reservoir; stirring and dissolving; add activated monomer and light trigger; stirring and dissolving; add assisted resin, filler, organic pigment and auxiliary agent; stirring and dissolving, is eventually adding defoamer, namely obtains the UV solidification hydrofluoric acid resistant protection glue that can develop after mixing and stirring.
Compared with prior art, the UV of development disclosed in the present application solidifies hydrofluoric acid resistant protection glue and has the advantage that employing and glass surface have the protection glue of higher adhesion, effectively prevent the generation of demoulding phenomenon in processing procedure；The hydrofluoric acid resistant protection glue adopted has good anti-etching ability, and concrete advantage is as follows:
1) the application selects the one in bisphenol A epoxy acrylate, epoxy soybean oil acrylate, PU modified epoxy acrylate resin, anhydride modified epoxy acrylate or Chinese rose acid modified epoxy acrylic ester or its mixture as matrix resin; the developed UV making the present invention solidifies hydrofluoric acid resistant protection glue except having the feature of epoxy bond function admirable; also have both unsaturated polyester resin fast to solidify; quickly obtain working strength, obtain that there is high corrosion resistance polymer；
2) the application assisted resin is to add to adjust the bulk property of adhesive, compensate for matrix resin in hot strength, heatproof character, some of the aspect such as hardness is not enough, hence it is evident that improve the performance of the aspects such as the protection adhesivity of glue, heatproof；
3) hinge structure, the acrylate containing fluorine activated monomer that the application has also selected high surface, height is heat-resisting and highly corrosion resistant is good so that the curable adhesive of the present invention still remains good adhesive strength when hot and humid, high hydrofluoric acid concentration；
4) the developed UV that the application provides solidifies hydrofluoric acid resistant protection glue; there is the stickiness protecting glue more excellent than the hydrofluoric acid resistant of prior art; especially glass is had high adhesive strength, and hydrofluoric acid resistant etching performance is excellent, has broad application prospects.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearly understand, below in conjunction with case study on implementation, the present invention is further elaborated.Should be appreciated that specific embodiment described herein is only in order to explain the present invention, is not intended to limit the present invention.
The preparation method that the UV that can develop solidifies hydrofluoric acid resistant protection glue; comprise the following steps: according to quality proportioning by resin, activated monomer, light trigger, filler, auxiliary agent; and organic pigment stirs at the temperature lower than 30 DEG C, namely obtain the UV solidification hydrofluoric acid resistant protection glue that can develop.
Tested viscosity, if test result is unsatisfactory for the viscosity threshold set, then adjusts viscosity to described viscosity threshold, and the developed UV that namely viscosity threshold of described setting prepares solidifies the range of viscosities of hydrofluoric acid resistant protection glue.Viscosity be determine to develop UV solidify hydrofluoric acid resistant protection colloidality can major parameter, viscosity is too big, and the UV that is unfavorable for developing solidifies the coating of hydrofluoric acid resistant protection glue；And the too little impact causing the degree of cross linking cannot prevent Fluohydric acid. liquid not of viscosity and infiltration are thus corroding protected glass; therefore the UV that can develop solidifies hydrofluoric acid resistant and protects the viscosity of glue need to meet the viscosity threshold of setting; one is preferably carried out in mode, and viscosity threshold is set as 5000～40000mPa s.
Detailed description of the invention described herein only in order to explain the present invention, is not intended to limit the present invention.
The etch resistant performance that the UV that can develop solidifies hydrofluoric acid resistant protection glue is measured by the following method:
According to experimental program by the glue prepared by flat painting or/and spin coating mode is coated on the glass substrate cleaned up, the thickness of glued membrane, in 20～60m scope, is then added a cover Masker plate and is carried out UV exposure, and light exposure is 1500～2500mj/cm2, produce groove pattern, through inorganic alkali liquor develop (concentration is 0.04%KOH aqueous solution) remove the protection glue on groove, will really need the part of etching to decide completely, this segment glass substrate is completely exposed.Finally by the glass substrate after bake 20min on 100 DEG C of hot plates after development, make protection glued membrane organic principle cross-link further, the chemical reaction such as polymerization and solidify.Fluohydric acid. protection glued membrane plays the protective effect when etching to glass substrate, has the part of protecting film to be etched, and the part without protection glued membrane will be etched, and forms required groove.
The glass substrate scribbling protection glued membrane made is put into etching groove, and etching solution is the hydrofluoric acid solution of 40%, and etch temperature is 30 DEG C, and etch-rate is 5～6m/min, and etching period is 1～3h.Generally soaking etching, spray etching for etching big method, the time used by immersion way is longer, and it is higher to the anti-etching performance requirement of protection glued membrane to spray mode.The present embodiment adopts the mode of top spray to be etched.
Cleaning glass substrate after having etched, etching is carried out after terminating immediately, mainly: (one) terminates the carrying out of etching reaction, it is ensured that etching precision；(2) etching solution is removed to carry out in artificial following effect not by etching solution typhoid fever；The present embodiment takes the mode of top spray to clean the etching solution of glass baseplate surface.
Finally the glass substrate after etching is immersed in degumming film in the inorganic alkali liquor (concentration is 10%KOH aqueous solution) of temperature 60 C.
Embodiment 1
Each raw material composition that the UV that can develop in the present embodiment solidifies hydrofluoric acid resistant protection glue is as follows with proportioning (mass percent):
Bisphenol-A epoxy acrylic acid light-cured resin 50%, polyether based polyurethanes acrylate 20%, light trigger 3694.5%, dodecafluoroheptyl methacrylate 5%, trimethylolpropane tris (methyl) acrylate 5%, tetramethylolmethane three (methyl) acrylate 5%, filler 8%, auxiliary agent 2% and pigment P.R.2540.5%, be uniformly mixed and get final product.
Measure the etch resistant performance of this proved recipe case according to the method for testing of above-mentioned etch resistant performance, protecting film thickness is 35mm, etching period 1.5h, and etch depth is 0.45mm, degumming film time 30min.
Embodiment 2
Each raw material composition that the UV that can develop in the present embodiment solidifies hydrofluoric acid resistant protection glue is as follows with proportioning (mass percent):
Bisphenol-A epoxy acrylic acid light-cured resin 22%, PU modified epoxy acrylate resin 22%, aliphatic urethane acrylate 20%, light trigger 3696.5%, hexafluorobutyl acrylate 2%, dodecafluoroheptyl methacrylate 3%, trimethylolpropane tris (methyl) acrylate 10%, filler 9%, auxiliary agent 5% and pigment P.R.2540.5% are uniformly mixed and get final product.
Measure the etch resistant performance of this proved recipe case according to the method for testing of above-mentioned etch resistant performance, protecting film thickness is 60mm, etching period 3h, and etch depth is 1.10mm, degumming film time 75min.
Embodiment 3
Each raw material composition that the UV that can develop in the present embodiment solidifies hydrofluoric acid resistant protection glue is as follows with proportioning (mass percent):
Epoxy soybean oil acrylate 30%, anhydride modified epoxy acrylate 20%, aliphatic urethane acrylate 10%, amino acrylic resin 15%, light trigger 9073.5%, dodecafluoroheptyl methacrylate 5%, tetramethylolmethane three (methyl) acrylate 5%, filler 5%, auxiliary agent 6% and pigment P.G.360.5% are uniformly mixed and get final product.
Measure the etch resistant performance of this proved recipe case according to the method for testing of above-mentioned etch resistant performance, protecting film thickness is 40mm, etching period 2h, and etch depth is 0.65mm, degumming film time 60min.
Embodiment 4
Each raw material composition that the UV that can develop in the present embodiment solidifies hydrofluoric acid resistant protection glue is as follows with proportioning (mass percent):
Chinese rose acid modified epoxy acrylic ester 25%, anhydride modified epoxy acrylate 22%, aliphatic urethane acrylate 10%, PBAA ester 10%, amino acrylic resin 5%, light trigger 1843.5%, dodecafluoroheptyl methacrylate 5%, glycerol dimaleate 5%, dipentaerythritol six maleate 5%, filler 5%, auxiliary agent 4% and pigment P.G.360.5% are uniformly mixed and get final product.
Measure the etch resistant performance of this proved recipe case according to the method for testing of above-mentioned etch resistant performance, protecting film thickness is 25mm, etching period 1h, and etch depth is 0.35mm, degumming film time 30min.
Embodiment 5
Each raw material composition that the UV that can develop in the present embodiment solidifies hydrofluoric acid resistant protection glue is as follows with proportioning (mass percent):
Chinese rose acid modified epoxy acrylic ester 25%, epoxy soybean oil acrylate 20%, aliphatic urethane acrylate 12%, polyether based polyurethanes acrylate 8%, amino acrylic resin 5%, light trigger 1843.5%, hexafluorobutyl acrylate 2%, dodecafluoroheptyl methacrylate 5%, trimethylolpropane tris maleate 5%, dipentaerythritol six maleate 5%, filler 5%, auxiliary agent 4% and pigment P.G.360.5% are uniformly mixed and get final product.
Measure the etch resistant performance of this proved recipe case according to the method for testing of above-mentioned etch resistant performance, protecting film thickness is 55mm, etching period 2h, and etch depth is 0.85mm, degumming film time 60min.
Embodiment 6
Each raw material composition that the UV that can develop in the present embodiment solidifies hydrofluoric acid resistant protection glue is as follows with proportioning (mass percent):
Bisphenol-A epoxy acrylic acid light-cured resin 30%, epoxy soybean oil acrylate 15%, aliphatic urethane acrylate 15%, amino acrylic resin 12%, light trigger 1844.5%, hexafluorobutyl acrylate 2%, dodecafluoroheptyl methacrylate 5%, trimethylolpropane tris maleate 5%, trimethylolpropane tris (methyl) acrylate 5%, filler 4%, auxiliary agent 2% and pigment P.G.360.5% are uniformly mixed and get final product.
Measure the etch resistant performance of this proved recipe case according to the method for testing of above-mentioned etch resistant performance, protecting film thickness is 42mm, etching period 1.5h, and etch depth is 0.45mm, degumming film time 50min.
Embodiment 7
Each raw material composition that the UV that can develop in the present embodiment solidifies hydrofluoric acid resistant protection glue is as follows with proportioning (mass percent):
Bisphenol-A epoxy acrylic acid light-cured resin 30%, Chinese rose acid modified epoxy acrylic ester 20%, polyether based polyurethanes acrylate 10%, amino acrylic resin 12%, light trigger 3694.5%, hexafluorobutyl acrylate 2%, hexanediol two (methyl) acrylate 5%, trimethylolpropane tris maleate 15%, filler 4%, auxiliary agent 2% and pigment P.G.360.5% are uniformly mixed and get final product.
Measure the etch resistant performance of this proved recipe case according to the method for testing of above-mentioned etch resistant performance, protecting film thickness is 35mm, etching period 2h, and etch depth is 0.88mm, degumming film time 70min.
Embodiment 8
Each raw material composition that the UV that can develop in the present embodiment solidifies hydrofluoric acid resistant protection glue is as follows with proportioning (mass percent):
Bisphenol-A epoxy acrylic acid light-cured resin 45%, amino acrylic resin 25%, light trigger TPO4.5%, hexafluorobutyl acrylate 2%, dodecafluoroheptyl methacrylate 5%, dicyclopentadiene acrylate 5%, propylene glycol two crotonates 5%, filler 6%, auxiliary agent 2% and pigment P.V.230.5% are uniformly mixed and get final product.
Measure the etch resistant performance of this proved recipe case according to the method for testing of above-mentioned etch resistant performance, protecting film thickness is 50mm, etching period 2.5h, and etch depth is 1mm, degumming film time 80min.
The above; being only the specific embodiment of the present invention, but protection scope of the present invention is not limited thereto, any those familiar with the art is in the technical scope that the invention discloses; change can be readily occurred in or replace, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with scope of the claims.
Claims (7)
1. the UV that can develop solidifies a hydrofluoric acid resistant protection glue, and by mass percentage, its composition includes: matrix resin 25～65%; assisted resin 15～35%, activated monomer 8～16%, the light trigger of 1～10%; filler 0.5-20%, auxiliary agent 0.5-10%, organic pigment 0.1～1%；
Described matrix resin be bisphenol A epoxy acrylate, epoxy soybean oil acrylate, PU modified epoxy acrylate resin, anhydride modified epoxy acrylate or Chinese rose acid modified epoxy acrylic ester or in one or both mixture, one or both the mixture in polyether based polyurethanes acrylate, epoxy acrylate, urethane acrylate, PBAA ester；
Described assisted resin is one or both the mixture in aliphatic urethane acrylate, amino acrylic resin, PBAA ester, polyester acrylate；
One or more in simple function group, difunctional or multi-functional acrylate containing fluorine activated monomer of described activated monomer, one or more in simple function group, difunctional or multi-functional vinyl compound activated monomer；
Described activated monomer is simple function group, difunctional or multi-functional acrylate containing fluorine activated monomer is the mixture of 1:1～1:5 in mass ratio with simple function group, difunctional or multi-functional vinyl compound activated monomer.
2. one according to claim 1 can develop UV solidify hydrofluoric acid resistant protection glue, it is characterised in that: the degree of functionality of described matrix resin be 2 and viscosity be 5500～45000mPa.s；The degree of functionality of described assisted resin be 2～6 and viscosity be 1500～15000mPa.s.
3. the UV that develops according to claim 1 solidifies hydrofluoric acid resistant protection glue composition; it is characterized in that: described acrylate containing fluorine activated monomer is selected from one or more in following substances: fluorinated acrylate selects hexafluorobutyl acrylate; Hexafluorobutyl mathacrylate; trifluoroethyl methacrylate; dodecafluoroheptyl methacrylate; dodecafluorhe-ptylacrylate, acrylic acid 19 fluorine ester；
Described vinyl compound includes at least (methyl) acrylate group.
4. one according to claim 1 can develop UV solidify hydrofluoric acid resistant protection glue, it is characterised in that: described filler is nano-TiO2。
5. the one according to claim 1 UV that can develop solidifies hydrofluoric acid resistant protection glue, it is characterised in that: described light trigger eliminates one or more the mixture in reaction mechanism light trigger, visible light initiator, radical photoinitiator selected from cracking reaction photoinitiator, hydrogen.
6. the one according to claim 5 UV that can develop solidifies hydrofluoric acid resistant protection glue, it is characterised in that: one or more in the following substances of described light trigger: the coordination compound of benzoin ether, benzil ketals, 1-Phenylethanone., acylphosphine oxide, benzophenone and tertiary amine, thioxanthone, the derivant of thioxanthone, double; two imidazoles, camphorquinone.
7. one according to claim 1 can develop UV solidify hydrofluoric acid resistant protection glue, it is characterised in that: described auxiliary agent is adhesion promoter, levelling agent, defoamer, stabilizer, and its mass ratio is 1:1:1:1.
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| CN105315946A (en) * | 2015-11-23 | 2016-02-10 | 苏州盖德精细材料有限公司 | Epoxy acrylate UV adhesive and preparation method thereof |
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| CN115746771A (en) * | 2022-10-28 | 2023-03-07 | 环晟光伏(江苏)有限公司 | Mask adhesive, preparation method thereof and manufacturing method of solar cell |
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| CN103666307B (en) * | 2013-12-31 | 2015-10-07 | 杭州大华塑业有限公司 | A kind of Acid-resistant protection film rubber belt |
| CN103865470B (en) * | 2014-02-12 | 2016-04-06 | 惠晶显示科技（苏州）有限公司 | A kind of photocuring edge sealing adhesive |
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