WO2023216931A1 - 一种热固型耐候保护涂层材料及其制备方法和用途 - Google Patents
一种热固型耐候保护涂层材料及其制备方法和用途 Download PDFInfo
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- WO2023216931A1 WO2023216931A1 PCT/CN2023/091671 CN2023091671W WO2023216931A1 WO 2023216931 A1 WO2023216931 A1 WO 2023216931A1 CN 2023091671 W CN2023091671 W CN 2023091671W WO 2023216931 A1 WO2023216931 A1 WO 2023216931A1
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- WIPO (PCT)
- Prior art keywords
- protective coating
- coating material
- resistant protective
- weather
- thermosetting
- Prior art date
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- 239000011253 protective coating Substances 0.000 title claims abstract description 83
- 239000000463 material Substances 0.000 title claims abstract description 73
- 229920001187 thermosetting polymer Polymers 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 30
- 239000003054 catalyst Substances 0.000 claims abstract description 29
- 239000003112 inhibitor Substances 0.000 claims abstract description 29
- 229910052751 metal Inorganic materials 0.000 claims abstract description 26
- 239000002184 metal Substances 0.000 claims abstract description 26
- 239000004094 surface-active agent Substances 0.000 claims abstract description 26
- 239000003960 organic solvent Substances 0.000 claims abstract description 23
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 20
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 20
- 239000012948 isocyanate Substances 0.000 claims abstract description 11
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 11
- 239000011347 resin Substances 0.000 claims description 22
- 229920005989 resin Polymers 0.000 claims description 22
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 18
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 11
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 10
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 claims description 6
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 6
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 6
- LZCLXQDLBQLTDK-UHFFFAOYSA-N ethyl 2-hydroxypropanoate Chemical compound CCOC(=O)C(C)O LZCLXQDLBQLTDK-UHFFFAOYSA-N 0.000 claims description 6
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- LCTONWCANYUPML-UHFFFAOYSA-N Pyruvic acid Chemical compound CC(=O)C(O)=O LCTONWCANYUPML-UHFFFAOYSA-N 0.000 claims description 4
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 claims description 4
- AYLRODJJLADBOB-QMMMGPOBSA-N methyl (2s)-2,6-diisocyanatohexanoate Chemical compound COC(=O)[C@@H](N=C=O)CCCCN=C=O AYLRODJJLADBOB-QMMMGPOBSA-N 0.000 claims description 4
- 229920001296 polysiloxane Polymers 0.000 claims description 4
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical group CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 3
- 229940116333 ethyl lactate Drugs 0.000 claims description 3
- TYEYBOSBBBHJIV-UHFFFAOYSA-N 2-oxobutanoic acid Chemical compound CCC(=O)C(O)=O TYEYBOSBBBHJIV-UHFFFAOYSA-N 0.000 claims description 2
- KXBFLNPZHXDQLV-UHFFFAOYSA-N [cyclohexyl(diisocyanato)methyl]cyclohexane Chemical compound C1CCCCC1C(N=C=O)(N=C=O)C1CCCCC1 KXBFLNPZHXDQLV-UHFFFAOYSA-N 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 claims description 2
- -1 acrylic polyol Chemical class 0.000 claims description 2
- 229920003180 amino resin Polymers 0.000 claims description 2
- FFGHLLOLFQHABK-UHFFFAOYSA-L dibutyltin(2+);dodecane-1-thiolate Chemical compound CCCCCCCCCCCCS[Sn](CCCC)(CCCC)SCCCCCCCCCCCC FFGHLLOLFQHABK-UHFFFAOYSA-L 0.000 claims description 2
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 2
- 150000002576 ketones Chemical group 0.000 claims description 2
- 229920005862 polyol Polymers 0.000 claims description 2
- 229940107700 pyruvic acid Drugs 0.000 claims description 2
- 235000010290 biphenyl Nutrition 0.000 claims 1
- 239000004305 biphenyl Substances 0.000 claims 1
- 125000006267 biphenyl group Chemical group 0.000 claims 1
- XJRAOMZCVTUHFI-UHFFFAOYSA-N isocyanic acid;methane Chemical compound C.N=C=O.N=C=O XJRAOMZCVTUHFI-UHFFFAOYSA-N 0.000 claims 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 claims 1
- 239000012974 tin catalyst Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 21
- 238000000576 coating method Methods 0.000 description 38
- 239000011248 coating agent Substances 0.000 description 35
- 238000012360 testing method Methods 0.000 description 34
- 238000003860 storage Methods 0.000 description 22
- 238000002156 mixing Methods 0.000 description 19
- 238000001723 curing Methods 0.000 description 18
- 239000003292 glue Substances 0.000 description 12
- 239000000758 substrate Substances 0.000 description 10
- 239000007787 solid Substances 0.000 description 9
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 6
- 238000007665 sagging Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000010907 mechanical stirring Methods 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 239000004721 Polyphenylene oxide Substances 0.000 description 4
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 4
- 239000004205 dimethyl polysiloxane Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 4
- 229920000570 polyether Polymers 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- 238000002310 reflectometry Methods 0.000 description 3
- 238000002834 transmittance Methods 0.000 description 3
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000004744 fabric Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000011241 protective layer Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 230000035939 shock Effects 0.000 description 2
- 239000011780 sodium chloride Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002087 whitening effect Effects 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 229910001252 Pd alloy Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000003848 UV Light-Curing Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- XPPWAISRWKKERW-UHFFFAOYSA-N copper palladium Chemical compound [Cu].[Pd] XPPWAISRWKKERW-UHFFFAOYSA-N 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000012985 polymerization agent Substances 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000011417 postcuring Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Definitions
- thermosetting weather-resistant protective coating material and its preparation method and use The entire contents are incorporated herein by reference.
- the invention belongs to the field of chemical protective coating materials, and specifically relates to a thermosetting weather-resistant protective coating material and its preparation method and use.
- Touch sensors are a cost-effective choice for realizing touch functions in electronic terminal products such as laptops, vehicles, medical, smart business and smart homes.
- touch sensors based on various materials ITO, nano-silver, metal mesh, etc.
- ITO indium-oxide-semiconductor
- nano-silver nano-silver
- metal mesh metal mesh
- the touch sensor is attached to the display panel through OCA glue and is the functional device closest to the external environmental medium in the display module. Therefore, the weather resistance of the touch sensor is one of the key indicators.
- module manufacturers assemble touch screens, there is a risk of scratching precision conductive circuits after removing the adhered polyurethane (PU) protective film. Solvents are also used to clean the sensor surface, so touch control is required.
- the device surface has good solvent resistance.
- the purpose of the present invention is to overcome the shortcomings of protective coating materials in the prior art that usually cannot combine lightness and thinness, weather resistance and/or solvent resistance, and provide a thermosetting weather-resistant protective coating material that can pass
- a variety of coating methods are prepared on the surface of metal mesh devices with a thickness of 1-3 ⁇ m. While ensuring lightness and thinness, it not only improves the solvent resistance of the device, protects precision circuits from damage, but also can pass strict weather resistance tests. , thereby improving the module factory’s process yield and reducing production costs.
- the present invention provides a thermosetting weather-resistant protective coating material
- the thermosetting weather-resistant protective coating material includes a separate first component and a second component, wherein the The first component includes an acrylic resin, a catalyst, a polymerization inhibitor, a surfactant and an organic solvent, and the second component includes an isocyanate curing agent.
- thermosetting weather-resistant protective coating material provided by the present invention is a two-component thermosetting weather-resistant protective coating material.
- the first component and the second component can be placed separately, for example in different containers or placed in different compartments of the same container. However, during use, the first component and the second component can be mixed directly, and spray coating, dipping, etc. can be selected according to the conditions of the substrate.
- Various coating processes such as coating, dimpling, and slit coating are applied to various substrate surfaces, such as metals, polymer films, and glass surfaces.
- the composition ratio of each component of the present invention there is no strict limit on the composition ratio of each component of the present invention. It can be adjusted according to the knowledge and experiments of those skilled in the art and actual needs, as long as it can meet the desired thinning, solvent resistance and weather resistance. Sex and other aspects are all required.
- the contents of the acrylic resin, catalyst, polymerization inhibitor, surfactant and isocyanate curing agent can be 20 respectively.
- the term "acrylic resin” is a general term for polymers of acrylic acid, methacrylic acid and their derivatives.
- the acrylic resin can be selected from one or more of acrylic polyol resin and acrylic amino resin; more preferably, the acrylic resin can be T2303 resin of Shanghai Hanfei Company (solid content 40%). According to research, the acrylic resin can exhibit excellent optical properties, good adhesion to the substrate, good adhesion to electroplated metal, and good flexibility to the coating film, and can also have excellent alcohol resistance. properties, excellent durability, etc.
- the term "catalyst” refers to a catalyst used to catalyze the reaction of acrylate and curing agent.
- the catalyst may be an organotin catalyst; more preferably, the catalyst may be selected from one of dibutyltin dilaurate and di(dodecylthio)dibutyltin or Various.
- the term "polymerization inhibitor” refers to auxiliaries which are generally used to prevent polymerization from proceeding.
- the polymerization inhibitor is a ketone acidic organic solvent; more preferably, the polymerization inhibitor can be selected from one of acetylacetone, 2-ketobutyric acid and pyruvic acid or Various.
- the main function of the polymerization inhibitor is to reduce the side reactions after mixing the A/B components. At the same time, it can alleviate the sagging phenomenon of the slit lip during slit coating, and the polymerization inhibitor is an organic solvent. , can be completely volatilized after heating.
- the term “surfactant” refers to a substance that can significantly reduce the surface tension of a target solution.
- the surfactant may include one or more of modified silicone and acrylate leveling agents.
- the term “leveling agent” refers to a commonly used coating additive, which can promote the coating to form a flat, smooth and uniform coating film during the drying and film-forming process. It can effectively reduce the surface tension of the coating fluid and improve its flow. Smoothness and uniformity.
- the modified silicone leveling agent can be selected from one or more of BYK333 and BYK3550; and the acrylic leveling agent can be selected from BYK3560 and BYK3565. of one or more.
- the type of organic solvent is not particularly limited as long as it has good solubility to other components in the thermosetting weather-resistant protective coating material of the present invention.
- the organic solvent may be selected from one or more of ethyl lactate, butyl acetate, ethyl acetate and ethyl propionate, but is not limited thereto.
- the isocyanate curing agent can be selected from toluene diisocyanate (TDI), isophorone diisocyanate (IPDI), diphenylmethane diisocyanate (MDI) ), one or more of dicyclohexylmethane diisocyanate (HMDI), hexamethylene diisocyanate (HDI) and lysine diisocyanate (LDI).
- TDI toluene diisocyanate
- IPDI isophorone diisocyanate
- MDI diphenylmethane diisocyanate
- HMDI dicyclohexylmethane diisocyanate
- HDI hexamethylene diisocyanate
- LLI lysine diisocyanate
- the present invention also provides a method for preparing the above-mentioned thermosetting weather-resistant protective coating material, which includes: mixing a predetermined proportion of acrylic resin, catalyst, polymerization inhibitor, surfactant and organic solvent To obtain the first component, and weigh a predetermined proportion of isocyanate curing agent as the second component, to obtain the thermosetting weather-resistant protective coating material.
- thermosetting weather-resistant protective coating material of the present invention is a two-component thermosetting weather-resistant protective coating material. Therefore, during the preparation process, the first component and the second component are usually prepared separately. For subsequent further use, it should be understood that the preparation method of the present invention does not exclude the possibility of directly mixing and preparing the first component and the second component immediately before using the thermosetting weather-resistant protective coating material of the present invention, and then The thermosetting weather-resistant protective coating material of the present invention is immediately used for subsequent processes.
- the predetermined ratio can be set with reference to the above ratios for each component.
- the predetermined ratio can be proportional to the content of each component in the thermosetting weather-resistant protective coating material, such as based on the heat
- the predetermined proportions of polymerization agent, surfactant and isocyanate curing agent are 20-35% by weight, 0.5-5% by weight, 10-20% by weight, 0.1-0.5% by weight and 2-10% by weight respectively, and the rest are organic Solvent.
- thermosetting weather-resistant protective coating material which includes the following steps:
- Step 1 Preparation of the first component: Weigh the resin, catalyst, polymerization inhibitor, organic solvent and surfactant respectively according to predetermined weight percentages, then slowly add the resin to the solvent, turn on mechanical stirring, and finally add the polymerization inhibitor in sequence , catalyst and surfactant, mixed evenly to obtain a clear and transparent main resin solution;
- Step 2 Weigh the second component: Weigh the curing agent according to the proportion of complete reaction between the -OH or -NH2 group in the acrylic resin and the -NCO group in the curing agent;
- Step 3 Mixing of the first component and the second component: Place the first component in storage tank 1, place the second component in storage tank 2, storage tank 1 and storage tank 2 It flows into the mixing tank according to a certain flow ratio (that is, the flow ratio to achieve predetermined weight ratio mixing), and finally the glue in the mixing tank is pumped to the coating head.
- a certain flow ratio that is, the flow ratio to achieve predetermined weight ratio mixing
- the present invention also provides the use of the above-mentioned thermosetting weather-resistant protective coating material for a metal grid touch sensor.
- the technical solution of the present invention at least includes one or more of the following advantages:
- thermosetting weather-resistant protective coating material provided by the present invention has a low viscosity and can be applied to the surface of the protective element in a variety of coating methods, including but not limited to shower coating, dip coating, blade coating, and slit coating. Cloth, micro-gravure coating, and depending on the type of device, double-sided or single-sided coating can be selected;
- thermosetting weather-resistant protective coating material provided by the present invention has a wide range of matching substrates and good adhesion, and can be used with polymer material substrates (PET, COP, CPI, PMMA, PC-ABC); metal layers (including Copper, copper-palladium alloy); glass adhesion can reach 5B;
- thermosetting weather-resistant protective coating material provided by the present invention can achieve the above effect when the thickness after drying is 1-3 ⁇ m, without increasing the thickness of the touch sensor body, and does not require superimposed protection when assembled into the touch screen.
- membrane the thickness of the whole machine is also lighter and thinner;
- thermosetting weather-resistant protective coating material provided by the present invention has good solvent resistance on the surface after drying, and can be used in polar/non-polar solvents such as absolute ethanol, n-heptane, n-hexane, and cyclohexane.
- polar/non-polar solvents such as absolute ethanol, n-heptane, n-hexane, and cyclohexane.
- thermosetting weather-resistant protective coating material provided by the present invention has better optical properties after drying.
- the transmittance of the metal grid sensor after double-sided coating of the coating is improved.
- the reflectivity and haze decreased, and the chromaticity b* did not change significantly;
- thermosetting weather-resistant protective coating material provided by the present invention can fill the uneven surface structure on the substrate or sensor when coated on the touch sensor, thereby reducing the risk of touch damage. control sensor haze and
- thermosetting weather-resistant protective coating material provided by the present invention has relatively good weather resistance after drying. It can meet different requirements of weather resistance standards without printing insulating ink, and reduces the process of printing and UV curing insulating ink. , improve efficiency and reduce costs;
- the metal grid sensor coated with the thermosetting weather-resistant protective coating material provided by the present invention can pass the weather resistance test after being assembled into a touch module, including: High temperature and high humidity (85°C, 85% humidity for 240h; 60°C, 90% humidity for 240h), hot and cold shock (low temperature -40°C (20min) ⁇ high temperature 65°C (20min); 100 cycles), UV aging ( UV test uses UVA340 lamp; 0.77W/(m2 ⁇ nm)), salt spray test (35°C, sodium chloride 5%, pH 6.5-7.2, 96h), high temperature storage (85°C; 240h).
- thermosetting weather-resistant protective coating material provided by the present invention react quickly, and the reaction is basically complete when offline, which greatly shortens the later aging reaction time. At the same time It also plays a role in prompting the wet film to dry quickly;
- the thermosetting weather-resistant protective coating material provided by the present invention has a wide range of solvents available for selection.
- the solvent can be selected according to the actual conditions of the process equipment (such as coating machine line speed, oven temperature, etc.), such as ethyl lactate as the diluent.
- the coating liquid When used as a solvent, the coating liquid has high wettability to the PET substrate and metal mesh, which can prevent glue overflow at the edge of the substrate; it can also increase the dry film thickness of the protective coating on the metal mesh.
- thermosetting weather-resistant protective coating material S1 The types and contents of each component in the thermosetting weather-resistant protective coating material S1 are as follows:
- Acrylic resin 27.5% by weight (Shanghai Hanfei Company T2303 resin);
- Catalyst 2% by weight (dibutyltin dilaurate);
- Polymerization inhibitor 10% by weight (acetylacetone);
- Surfactant 0.2% by weight (polyether modified dimethylpolysiloxane, BYK333);
- Curing agent 6.5% by weight (hexamethylene diisocyanate (HDI)).
- thermosetting weather-resistant protective coating material S1 is prepared as follows:
- Step 1 Preparation of the first component: Weigh the resin, catalyst, polymerization inhibitor, organic solvent and surfactant respectively according to the above weight percentages, then slowly add the resin to the solvent, turn on mechanical stirring, and finally add the polymerization inhibitor in sequence , catalyst and surfactant, mixed evenly to obtain a clear and transparent main resin solution;
- Step 2 Weigh the second component: Weigh the HDI curing agent according to the weight percentage as above;
- Step 3 Mixing of the first component and the second component: Place the first component in storage tank 1, place the second component in storage tank 2, storage tank 1 and storage tank 2 Flow into the mixing tank at a flow ratio of 93.5:6.5, and finally pump the glue in the mixing tank to the coating head.
- thermosetting weather-resistant protective coating material was 18.9%. It was applied on the surface of the metal grid through slit coating and baked in an oven at 100°C for 2 minutes to obtain a dry film thickness of 3 ⁇ m.
- thermosetting weather-resistant protective coating material S2 The types and contents of each component in the thermosetting weather-resistant protective coating material S2 are as follows:
- Acrylic resin 40.5% by weight (Shanghai Hanfei Company T2303 resin);
- Catalyst 2% by weight (dibutyltin dilaurate);
- Polymerization inhibitor 10% by weight (acetylacetone);
- Surfactant 0.2% by weight (polyether modified dimethylpolysiloxane, BYK333);
- Curing agent 9.6% by weight (hexamethylene diisocyanate (HDI)).
- thermosetting weather-resistant protective coating material S2 is prepared as follows:
- Step 1 Preparation of the first component: Weigh the resin, catalyst, polymerization inhibitor, organic solvent and surfactant respectively according to the above weight percentages, then slowly add the resin to the solvent, turn on mechanical stirring, and finally add the polymerization inhibitor in sequence , catalyst and surfactant, mixed evenly to obtain a clear and transparent main resin solution;
- Step 2 Weigh the second component: Weigh the HDI curing agent according to the weight percentage as above;
- Step 3 Mixing of the first component and the second component: Place the first component in storage tank 1, place the second component in storage tank 2, storage tank 1 and storage tank 2 Flow into the mixing tank at a flow ratio of 90.4:9.6, and finally pump the glue in the mixing tank to the coating head.
- thermosetting weather-resistant protective coating material The solid content of the obtained thermosetting weather-resistant protective coating material is 27%. It is coated on the surface of the metal grid through slit coating and baked in an oven at 100°C for 2 minutes to obtain a dry film thickness of 3 ⁇ m.
- thermosetting weather-resistant protective coating material S3 The types and contents of each component in the thermosetting weather-resistant protective coating material S3 are as follows:
- Acrylic resin 16.5% by weight (Shanghai Hanfei Company T2303 resin);
- Catalyst 2% by weight (dibutyltin dilaurate);
- Polymerization inhibitor 10% by weight (acetylacetone);
- Surfactant 0.2% by weight (polyether modified dimethylpolysiloxane, BYK333);
- Curing agent 4.3% by weight (hexamethylene diisocyanate (HDI)).
- thermosetting weather-resistant protective coating material S3 is prepared as follows:
- Step 1 Preparation of the first component: Weigh the resin, catalyst, polymerization inhibitor, organic solvent and surfactant respectively according to the above weight percentages, then slowly add the resin to the solvent, turn on mechanical stirring, and finally add the polymerization inhibitor in sequence , catalyst and surfactant, mixed evenly to obtain a clear and transparent main resin solution;
- Step 2 Weigh the second component: Weigh the HDI curing agent according to the weight percentage as above;
- Step 3 Mixing of the first component and the second component: Place the first component in storage tank 1, place the second component in storage tank 2, storage tank 1 and storage tank 2 Flow into the mixing tank at a flow ratio of 95.7:4.3, and finally pump the glue in the mixing tank to the coating head.
- thermosetting weather-resistant protective coating material The solid content of the obtained thermosetting weather-resistant protective coating material was 12.6%. It was applied on the surface of the metal grid through slit coating and baked in an oven at 100°C for 2 minutes to obtain a dry film thickness of 3 ⁇ m.
- thermosetting weather-resistant protective coating material D1 The types and contents of each component in the thermosetting weather-resistant protective coating material D1 are as follows:
- Acrylic resin 27.5% by weight (Shanghai Hanfei Company T2303 resin);
- Catalyst 2% by weight (dibutyltin dilaurate);
- Surfactant 0.2% by weight (polyether modified dimethylpolysiloxane, BYK333);
- Curing agent 6.5% by weight (hexamethylene diisocyanate (HDI)).
- thermosetting weather-resistant protective coating material D1 is prepared as follows:
- Step 1 Preparation of the first component: Weigh the resin, catalyst, polymerization inhibitor, organic solvent and surfactant respectively according to the above weight percentages, then slowly add the resin to the solvent, turn on mechanical stirring, and finally add the polymerization inhibitor in sequence , catalyst and surfactant, mixed evenly to obtain a clear and transparent main resin solution;
- Step 2 Weigh the second component: Weigh the HDI curing agent according to the weight percentage as above;
- Step 3 Mixing of the first component and the second component: Place the first component in storage tank 1, place the second component in storage tank 2, storage tank 1 and storage tank 2 Flow into the mixing tank at a flow ratio of 93.5:6.5, and finally pump the glue in the mixing tank to the coating head.
- thermosetting weather-resistant protective coating material was 18.9%. It was applied on the surface of the metal grid through slit coating and baked in an oven at 100°C for 2 minutes to obtain a dry film thickness of 3 ⁇ m.
- thermosetting weather-resistant protective coating materials obtained in Examples 1-4 and Comparative Example 1 are summarized in Table 1 below:
- thermosetting weather-resistant protective coating material obtained in Example 1 was selected for subsequent weathering aging testing.
- connection port on the FPC and the metal conductive film is hot-pressed and bound through ACF glue.
- a destructive test is performed using a tensile tester. When the FPC falls off from the metal grid conductive film, the force displayed on the pull gauge is defined as the pull-out force. When the pull-out force is greater than 500g/cm, the test is passed. The results are shown in Table 2 below.
- the test items include: high temperature and high humidity (85°C, 85% humidity for 240h; 60°C, 90% humidity Humidity 240h), hot and cold shock (low temperature -40°C (20min) ⁇ high temperature 65°C (20min); 100 cycles), UV aging (UV test with UVA340 lamp; 0.77W/(m2 ⁇ nm), light/temperature 60 °C ⁇ 2.5 (4h); condensation/temperature 50°C (4h), 25 cycles), salt spray test (35°C, sodium chloride 5%, pH 6.5-7.2, 96h, after taking out, store the sample at 25°C-35 °C, humidity 30%-60% environment for 24h), high temperature storage (85°C: 240h), if the electrical test before and after the weather resistance test passes, the weather resistance test passes.
- Table 2 The results are shown in Table 2 below.
- thermosetting weather-resistant protective coating material of Example 1 prepared by the formula of the present invention has better performance in solvent resistance, dyne value, adhesion, optical properties, and weather resistance.
- the results of the sex test all passed. That is to say, the thermosetting weather-resistant protective coating material of the present invention can simultaneously meet the requirements for device thinning, solvent resistance, and weather resistance, and therefore has excellent performance when applied to metal grid touch sensors. .
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Abstract
本发明提供了一种热固型耐候保护涂层材料及其制备方法和用途，所述热固型耐候保护涂层材料包含分开的第一组分和第二组分，其中所述第一组分包含丙烯酸树脂、催化剂、阻聚剂、表面活性剂和有机溶剂，并且所述第二组分包含异氰酸酯类固化剂。由于本发明的热固型耐候保护涂层材料能够同时满足实现器件轻薄化、耐溶剂性及耐候性等多方面的要求，并且相对节约成本、产品良率高，因此在应用于金属网格触控传感器时具备优异的性能。
Description
本申请要求于2022年05月07日提交中国专利局、申请号为2022104949528、发明名称为“一种热固型耐候保护涂层材料及其制备方法和用途”的中国专利申请的优先权，其全部内容通过引用结合在本申请中。
本发明属于化学保护涂层材料领域，具体地，涉及一种热固型耐候保护涂层材料及其制备方法和用途。
触控传感器是笔电、车载、医疗、智能商务和智能家居等电子终端产品实现触控功能的高性价比选择。目前基于各种材质(ITO，纳米银，金属网格等)的触控传感器得到广泛研究，其中堆叠结构为外挂式(触控组件叠构在显示屏组件上侧)的触控屏因适配大屏化、灵敏度高而得到越来越多的关注。
外挂式结构中触控传感器通过OCA胶贴附于显示面板之上，是显示模组里最接近外界环境介质的功能性器件，因此触控传感器的耐候性能是关键指标之一。模组厂商在组装的触控屏的过程中，去除贴合的聚氨酯(PU)保护膜后制程中存在划伤精密导电线路的风险，也会使用溶剂对传感器进行表面清洁，因此需要要求触控器件表面具有较好的耐溶剂性。
因此，急需开发一种能够同时满足实现器件轻薄化、耐溶剂性及耐候性等都方面要求的保护涂层材料。
发明内容
本发明的目的在于克服现有技术中的保护涂层材料通常无法兼具轻薄化、耐候性和/或耐溶剂性的缺陷，提供了一种热固型耐候保护涂层材料，该材料可以通过多种涂布方式以1-3μm的厚度制备于金属网格器件表面，在保证轻薄化的同时，不仅提高了器件的耐溶剂性，保护精密线路不受损伤，而且可以通过严格的耐候性测试，从而提升了模组厂制程良率，降低了生产成本。
为了实现上述目的，在一方面，本发明提供了一种热固型耐候保护涂层材料，所述热固型耐候保护涂层材料包含分开的第一组分和第二组分，其中所述第一组分包含丙烯酸树脂、催化剂、阻聚剂、表面活性剂和有机溶剂，并且所述第二组分包含异氰酸酯类固化剂。
本发明提供的热固型耐候保护涂层材料是一种双组分热固型耐候保护涂层材料，在使用前，所述第一组分和所述第二组分可以分开放置，例如置于不同的容器中或置于同一容器的不同隔室中，然而在使用时，可以将所述第一组分和所述第二组分直接混合，并根据基材的状况选择淋涂、浸涂、微凹、狭缝涂布等多种涂布工艺施用于各种基材表面，例如金属、高分子薄膜及玻璃表面等。
根据本发明，对本发明的各组分中的组成比例没有严格限制，可以根据本领域技术人员的知识和实验以及实际需要来进行调整，只要其能够符合所期望的轻薄化、耐溶剂性及耐候性等都方面要求即可。在本发明的一个优选实施方式中，基于所述热固型耐候保护涂层材料的总重量，所述丙烯酸树脂、催化剂、阻聚剂、表面活性剂和异氰酸酯类固化剂的含量可以分别为20-35重量％(例如20重量％、22重量％、25重量％、27重量％、30重量％、32重量％或35重量％等)、0.5-5重量％(0.5重量％、1重量％、2重量％、3重量％、4重量％或5重量％等)、10-20重量％(10重量％、12重量％、14重量％、16重量％、18重量％或20重量％)、0.1-0.5重量％(0.1重量％、0.2重量％、0.3重量％、0.4重量％
或0.5重量％)和2-10重量％(2重量％、3重量％、5重量％、7重量％、8重量％或10重量％等)，并且其余为有机溶剂，但不限于此。
对于第一组分，根据本发明，术语“丙烯酸树脂”是丙烯酸、甲基丙烯酸及其衍生物聚合物的总称。在本发明的一个优选实施方式中，所述丙烯酸树脂可以选自丙烯酸多元醇树脂和丙烯酸氨基树脂中的一种或多种；更优选地，所述丙烯酸树脂可以为上海翰飞公司的T2303树脂(固含量40％)。根据研究发现，所述丙烯酸树脂可以对涂膜的特性表现为优良的光学性能、对基材的良好附着力、对电镀金属附着力佳，以及良好的柔韧性，并且还可以具有优良的耐醇性、极佳的耐久性等。
根据本发明，术语“催化剂”是指用于催化丙烯酸酯与固化剂进行反应的催化剂。在本发明的一个优选实施方式中，所述催化剂可以为有机锡催化剂；更优选地，所述催化剂可以选自二月桂酸二丁基锡和二(十二烷硫基)二丁基锡中的一种或多种。
根据本发明，术语“阻聚剂”是指通常用于防止聚合作用进行的助剂。在本发明的一个优选实施方式中，所述阻聚剂为酮类酸性有机溶剂；更优选地，所述阻聚剂可以选自乙酰丙酮、2-酮丁酸和丙酮酸中的一种或多种。在本发明中，阻聚剂的作用主要为减少A/B组分混合后的副反应，同时在狭缝涂布时可以缓解狭缝唇口的流挂现象，并且该阻聚剂为有机溶剂，加热后可完全挥发。
根据本发明，术语“表面活性剂”是指是能使目标溶液表面张力显著下降的物质。表面活性剂的种类有很多种，在本发明的一个实施方式中，所述表面活性剂可以包含改性有机硅类和丙烯酸酯类流平剂中的一种或多种。其中，术语“流平剂”是指一种常用的涂料助剂，它能促使涂料在干燥成膜过程中形成一个平整、光滑、均匀的涂膜，能有效降低涂饰液表面张力，提高其流平性和均匀性。
在本发明的一个优选实施方式中，所述改性有机硅类流平剂可以选自BYK333和BYK3550中的一种或多种；并且所述丙烯酸酯类流平剂可以选自BYK3560和BYK3565中的一种或多种。
根据本发明，对有机溶剂的种类没有特别限制，只要其能够对本发明的热固型耐候保护涂层材料中的其他组分具有良好的溶解性即可。在本发明的一个实施方式中，所述有机溶剂可以选自乳酸乙酯、乙酸丁酯、乙酸乙酯和丙酸乙酯中的一种或多种，但不限于此。
对于第二组分，在本发明的一个优选实施方式中，所述异氰酸酯类固化剂可以选自甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)、二苯基甲烷二异氰酸酯(MDI)、二环己基甲烷二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HDI)和赖氨酸二异氰酸酯(LDI)中的一种或多种。
在另一方面，本发明还提供了一种用于制备上述热固型耐候保护涂层材料的方法，其包括：将预定比例的丙烯酸树脂、催化剂、阻聚剂、表面活性剂和有机溶剂混合以得到所述第一组分，并且称取预定比例的异氰酸酯类固化剂作为所述第二组分，以得到所述热固型耐候保护涂层材料。
如前所述，本发明的热固型耐候保护涂层材料是一种双组分热固型耐候保护涂层材料，因此在制备过程中，通常分别制备第一组分和第二组分，以备后续进一步使用，但应当理解的是，本发明的制备方法并不排除可以在即将使用本发明的热固型耐候保护涂层材料前直接混合制备第一组分和第二组分，然后立即使用本发明的热固型耐候保护涂层材料进行后续工艺。
对于预定比例，所述预定比例可以参照上文中针对各组分的比例来设置，例如所述预定比例可以与热固型耐候保护涂层材料中各组分的含量成正比，例如基于所述热固型耐候保护涂层材料的总重量，所述丙烯酸树脂、催化剂、阻
聚剂、表面活性剂和异氰酸酯类固化剂的预定比例分别为20-35重量％、0.5-5重量％、10-20重量％、0.1-0.5重量％和2-10重量％，并且其余为有机溶剂。
另外，本发明还提供了一种用于制备上述热固型耐候保护涂层材料的具体方法，其包括以下步骤：
步骤1.第一组分的配制：按预定重量百分比分别称量树脂、催化剂、阻聚剂、有机溶剂和表面活性剂，然后将树脂缓慢加入溶剂中，开启机械搅拌，最后依次加入阻聚剂、催化剂和表面活性剂，混合均匀后得澄清透明主体树脂溶液；
步骤2.第二组分的称取：按照丙烯酸树脂中-OH或-NH2基团和固化剂中-NCO基团完全反应的比例称取固化剂；以及
步骤3.第一组分和第二组分的混合：将第一组分放置于储料罐1中，将第二组分放置于储料罐2中，储料罐1和储料罐2按一定流量比(即实现预定重量比混合的流量比)流入混料罐中，最后将混料罐中的胶液泵送至涂头。
在另一方面，本发明还提供了上述热固型耐候保护涂层材料用于金属网格触控传感器的用途。
与现有的技术方案相比，本发明的技术方案至少包括以下优点中的一个或多个：
1)本发明提供的热固型耐候保护涂层材料具有较低的粘度，可匹配多种涂布方式涂覆到保护元件表面，包括且不限于淋涂、浸涂、刮涂、狭缝涂布、微凹涂布，并且根据器件的类型，可以选择双面或者单面涂布；
2)本发明提供的热固型耐候保护涂层材料所匹配的基底范围广，且粘附力好，与高分子材料基底(PET、COP、CPI、PMMA、PC-ABC)；金属层(包括铜、铜钯合金)；玻璃粘附力均可达到5B；
3)本发明提供的热固型耐候保护涂层材料在干燥后的厚度为1-3μm时即可达到所述效果，不增加触控传感器本体厚度，并且总装到触控屏中不需要叠加保护膜，整机厚度也更加轻薄；
4)本发明提供的热固型耐候保护涂层材料在干燥后表面具有较好的耐溶剂性，使用无水乙醇、正庚烷、正己烷、环己烷等极性/非极性溶剂中的一种或几种擦拭，表面均未出现溶解、发白、擦痕等现象；
5)本发明提供的热固型耐候保护涂层材料干燥后有较好的光学特性，双面涂布本涂层后的金属网格传感器，器件的光学特性中，透过率有所提升，反射率与雾度有所下降，色度b*无明显改变；
6)本发明提供的热固型耐候保护涂层材料除本身具有较低的雾度外，涂布在触控传感器上时，能够填充基材上或者传感器上凹凸的表面结构，从而可以降低触控传感器的雾度以及
7)本发明提供的热固型耐候保护涂层材料在干燥后具有相对较好的耐候性，不需要印刷绝缘油墨即可达到不同要求的耐候性标准，减少了印刷、UV固化绝缘油墨的工序，提升效率、降低成本；
8)本发明提供的热固型耐候保护涂层材料涂布本发明提供的热固型耐候保护涂层材料后的金属网格传感器在总装为触控模组后可以通过耐候性测试，包括：高温高湿(85℃，85％的湿度240h；60℃，90％的湿度240h),冷热冲击(低温-40℃(20min)～高温65℃(20min)；100个循环)，UV老化(UV测试用UVA340灯；0.77W/(m2·nm))，盐雾测试(35℃，氯化钠5％，pH 6.5-7.2，96h)，高温存储(85℃；240h)。
9)本发明提供的热固型耐候保护涂层材料中丙烯酸树脂和异氰酸酯类固化剂反应较快，下线时基本反应完全，大幅度缩短了后期的熟化反应时间，同时
也起到促使湿膜快速表干的作用；
10)本发明提供的热固型耐候保护涂层材料中溶剂可供选用范围广，可根据工艺设备实际情况(如涂布机线速、烘箱温度等)选用溶剂，如选用乳酸乙酯作为稀释溶剂时，涂液对PET基材和金属网格有较高的润湿性，可以防止基材边缘的溢胶现象；同时也可以增加金属网格上保护涂层的干膜厚度。
在本文中所披露的范围的端点和任何值都不限于该精确的范围或值，这些范围或值应当理解为包含接近这些范围或值的值。对于数值范围来说，各个范围的端点值之间、各个范围的端点值和单独的点值之间，以及单独的点值之间可以彼此组合而得到一个或多个新的数值范围，这些数值范围应被视为在本文中具体公开。
除非另有定义，本文使用的所有术语(包括技术和科学术语)具有与本发明所属领域的普通技术人员通常理解的相同的含义。还应当理解，诸如在通常使用的字典中定义的那些术语应该被解释为具有与它们在相关技术的上下文中的含义一致的含义，并且不会以理想化或过度形式化的含义来解释，除非在此明确地定义。
下面进一步结合实施例来阐述本发明；但这些实施例并不限制本发明的范围。除非另有声明，各实施例中所用的所有试剂材料均从商业途径获得；并且分析检测中所用仪器设备等均为本领域中通常使用的常规仪器设备。
实施例
实施例1
热固型耐候保护涂层材料S1中各组分的种类和含量如下：
第一组分
丙烯酸树脂：27.5重量％(上海翰飞公司T2303树脂)；
催化剂：2重量％(二月桂酸二丁基锡)；
阻聚剂：10重量％(乙酰丙酮)；
表面活性剂：0.2重量％(聚醚改性二甲基聚硅氧烷，BYK333)；
有机溶剂：53.8重量％(乙酸丁酯)；以及
第二组分
固化剂：6.5重量％(六亚甲基二异氰酸酯(HDI))。
热固型耐候保护涂层材料S1如下制备：
步骤1.第一组分的配制：按如上重量百分比分别称量树脂、催化剂、阻聚剂、有机溶剂和表面活性剂，然后将树脂缓慢加入溶剂中，开启机械搅拌，最后依次加入阻聚剂、催化剂和表面活性剂，混合均匀后得澄清透明主体树脂溶液；
步骤2.第二组分的称取：按照如上重量百分比称取HDI固化剂；以及
步骤3.第一组分和第二组分的混合：将第一组分放置于储料罐1中，将第二组分放置于储料罐2中，储料罐1和储料罐2按93.5：6.5的流量比流入混料罐中，最后将混料罐中的胶液泵送至涂头。
所得热固型耐候保护涂层材料的固含量为18.9％，通过狭缝涂布的施工方式涂布在金属网格表面，于100℃烘箱中烘烤2min，得到干膜厚度3μm。
实施例2
热固型耐候保护涂层材料S2中各组分的种类和含量如下：
第一组分
丙烯酸树脂：40.5重量％(上海翰飞公司T2303树脂)；
催化剂：2重量％(二月桂酸二丁基锡)；
阻聚剂：10重量％(乙酰丙酮)；
表面活性剂：0.2重量％(聚醚改性二甲基聚硅氧烷，BYK333)；
有机溶剂：37.7重量％(乙酸丁酯)；以及
第二组分
固化剂：9.6重量％(六亚甲基二异氰酸酯(HDI))。
热固型耐候保护涂层材料S2如下制备：
步骤1.第一组分的配制：按如上重量百分比分别称量树脂、催化剂、阻聚剂、有机溶剂和表面活性剂，然后将树脂缓慢加入溶剂中，开启机械搅拌，最后依次加入阻聚剂、催化剂和表面活性剂，混合均匀后得澄清透明主体树脂溶液；
步骤2.第二组分的称取：按照如上重量百分比称取HDI固化剂；以及
步骤3.第一组分和第二组分的混合：将第一组分放置于储料罐1中，将第二组分放置于储料罐2中，储料罐1和储料罐2按90.4：9.6的流量比流入混料罐中，最后将混料罐中的胶液泵送至涂头。
所得热固型耐候保护涂层材料的固含量为27％，通过狭缝涂布的施工方式涂布在金属网格表面，于100℃烘箱中烘烤2min，得到干膜厚度3μm。
实施例3
热固型耐候保护涂层材料S3中各组分的种类和含量如下：
第一组分
丙烯酸树脂：16.5重量％(上海翰飞公司T2303树脂)；
催化剂：2重量％(二月桂酸二丁基锡)；
阻聚剂：10重量％(乙酰丙酮)；
表面活性剂：0.2重量％(聚醚改性二甲基聚硅氧烷，BYK333)；
有机溶剂：67重量％(乙酸丁酯)；以及
第二组分
固化剂：4.3重量％(六亚甲基二异氰酸酯(HDI))。
热固型耐候保护涂层材料S3如下制备：
步骤1.第一组分的配制：按如上重量百分比分别称量树脂、催化剂、阻聚剂、有机溶剂和表面活性剂，然后将树脂缓慢加入溶剂中，开启机械搅拌，最后依次加入阻聚剂、催化剂和表面活性剂，混合均匀后得澄清透明主体树脂溶液；
步骤2.第二组分的称取：按照如上重量百分比称取HDI固化剂；以及
步骤3.第一组分和第二组分的混合：将第一组分放置于储料罐1中，将第二组分放置于储料罐2中，储料罐1和储料罐2按95.7：4.3的流量比流入混料罐中，最后将混料罐中的胶液泵送至涂头。
所得热固型耐候保护涂层材料的固含量为12.6％，通过狭缝涂布的施工方式涂布在金属网格表面，于100℃烘箱中烘烤2min，得到干膜厚度3μm。
对比例1
热固型耐候保护涂层材料D1中各组分的种类和含量如下：
第一组分
丙烯酸树脂：27.5重量％(上海翰飞公司T2303树脂)；
催化剂：2重量％(二月桂酸二丁基锡)；
表面活性剂：0.2重量％(聚醚改性二甲基聚硅氧烷，BYK333)；
有机溶剂：63.8重量％(乙酸丁酯)；以及
第二组分
固化剂：6.5重量％(六亚甲基二异氰酸酯(HDI))。
热固型耐候保护涂层材料D1如下制备：
步骤1.第一组分的配制：按如上重量百分比分别称量树脂、催化剂、阻聚剂、有机溶剂和表面活性剂，然后将树脂缓慢加入溶剂中，开启机械搅拌，最后依次加入阻聚剂、催化剂和表面活性剂，混合均匀后得澄清透明主体树脂溶液；
步骤2.第二组分的称取：按照如上重量百分比称取HDI固化剂；以及
步骤3.第一组分和第二组分的混合：将第一组分放置于储料罐1中，将第二组分放置于储料罐2中，储料罐1和储料罐2按93.5：6.5的流量比流入混料罐中，最后将混料罐中的胶液泵送至涂头。
所得热固型耐候保护涂层材料的固含量为18.9％，通过狭缝涂布的施工方式涂布在金属网格表面，于100℃烘箱中烘烤2min，得到干膜厚度3μm。
实施例1-4和对比例1得到的热固型耐候保护涂层材料的涂布性能汇总如下表1所示：
表1
由上表1可以看出，由于本发明的配方中丙烯酸树脂和固化剂的反应较快，为了防止狭缝涂布唇口的流挂现象，在配方中加入阻聚剂可有效控制涂液的固含量。更具体地，对比例1中无阻聚剂，因此唇口出现严重的流挂现象；实施案例2中涂液固含量较高，唇口出现部分流挂现象；实施例3中，涂液固含量
较低，唇口无流挂现象，但出现轻微湿膜膜面溢胶现象。
综合比较实施例1-4和对比例1的涂布性能后，由于实施例1中狭缝涂布唇口无流挂现象、湿膜膜面无溢胶现象、干膜无后期熟化，因此继续选择实施例1所得的热固型耐候保护涂层材料做后续耐候老化测试。
测试例1耐溶剂性测试
将提供配方涂液制备到基材上成为保护层后，使用蘸有无水乙醇、正庚烷、正己烷、环己烷溶剂的无尘布分别擦拭保护涂层表面20s，完成擦拭后，观察保护层状况，表面如未出现溶解、发白、擦痕等现象则通过耐溶剂性测试，反之则未通过。结果如下表2所示。
测试例2达因值测试
使用A.Shine DYNE TEST型号的达因笔测试涂层表面，达因值≥34mN/m即通过测试。结果如下表2所示。
测试例3附着力测试
(1)保护涂层与基材及金属层之间的附着力
在制备有金属网格图案的样品表面涂布制备2μm上述保护涂层干膜后，利用百格法测试保护涂层与基材区域及全镀铜区域之间的粘附力，具体步骤如下：使用百格刀在指定区域横竖划开，使用3M 610型号胶带黏贴，赶走气泡后，1-2s内撕除，观测测试百格区域涂层脱落情况，若无脱落，判定5B，则测试通过。结果如下表2所示。
(2)保护涂层与OCA胶之间的附着力
将所述保护涂层制备与金属网格导电膜正反表面，取两片上述带有保护涂层的导电膜，通过OCA胶将其贴合于一起，然后使用拉力计测试贴合的两层金属网格导电膜分离时的拉力值，大于1800gf/inch则测试通过。结果如下表2所
示。
(3)保护涂层与FPC之间的拉拔力
金属网格导电膜上下两面在完成上述保护涂层的制备后，将FPC与金属导电膜上的链接口通过ACF胶进行热压绑定，完成绑定后，使用拉力计进行破坏性测试，当FPC从金属网格导电膜上脱落时，拉力计上显示的力定义为拉拔力，当拉拔力大于500g/cm则测试通过。结果如下表2所示。
测试例4光学性能测试
使用lambda 850+UV紫外分光光度计测试涂布保护涂层前的双面金属网格产品的透过率，反射率，雾度，色度b*，对比两面涂布保护涂层后的样品数据，透过率下降不超过1％，反射率上升不超过1％，雾度上升不超过1％，色度b*上升不超过0.5，则达标。结果如下表2所示。
测试例5耐候性测试
双面涂布保护涂层的金属网格传感器总装为TP触控模组后，进行耐候可靠性测试，测试项目包括：高温高湿(85℃，85％的湿度240h；60℃，90％的湿度240h),冷热冲击(低温-40℃(20min)～高温65℃(20min)；100个循环)，UV老化(UV测试用UVA340灯；0.77W/(m2·nm)，光照/温度60℃±2.5(4h)；冷凝/温度50℃(4h)，25个循环)，盐雾测试(35℃，氯化钠5％，pH 6.5-7.2，96h，取出后即将样品保存25℃-35℃、湿度30％-60％的环境中24h)，高温存储(85℃：240h)，如耐候性测试前后电测均通过，则耐候性测试通过。结果如下表2所示。
表2
从表2的结果可知，与对比例相比，通过本发明配方制得的实施例1的热固型耐候保护涂层材料在进行耐溶剂性、达因值、粘附力、光学性能、耐候性测试时结果均通过。也就是说，本发明的热固型耐候保护涂层材料能够同时满足实现器件轻薄化、耐溶剂性及耐候性等都方面的要求，因此在应用于金属网格触控传感器时具备优异的性能。
以上详细描述了本发明的优选实施方式，但是，本发明并不限于上述实施方式中的具体细节，在本发明的技术构思范围内，可以对本发明的技术方案进行多种简单变型，这些简单变型均属于本发明的保护范围。
另外需要说明的是，在上述具体实施方式中所描述的各个具体技术特征，在不矛盾的情况下，可以通过任何合适的方式进行组合，为了避免不必要的重复，本发明对各种可能的组合方式不再另行说明。
此外，本发明的各种不同的实施方式之间也可以进行任意组合，只要其不
违背本发明的思想，其同样应当视为本发明所公开的内容。
Claims (14)
- 一种热固型耐候保护涂层材料，其特征在于，所述热固型耐候保护涂层材料包含分开的第一组分和第二组分，其中所述第一组分包含丙烯酸树脂、催化剂、阻聚剂、表面活性剂和有机溶剂，并且所述第二组分包含异氰酸酯类固化剂。
- 根据权利要求1所述的热固型耐候保护涂层材料，其中，基于所述热固型耐候保护涂层材料的总重量，所述丙烯酸树脂、催化剂、阻聚剂、表面活性剂和异氰酸酯类固化剂的含量分别为20-35重量％、0.5-5重量％、10-20重量％、0.1-0.5重量％和2-10重量％，并且其余为有机溶剂。
- 根据权利要求1或2所述的热固型耐候保护涂层材料，其中，所述丙烯酸树脂选自丙烯酸多元醇树脂和丙烯酸氨基树脂中的一种或多种。
- 根据权利要求1～3任一所述的热固型耐候保护涂层材料，其中，所述催化剂为有机锡催化剂。
- 根据权利要求1～4任一所述的热固型耐候保护涂层材料，所述催化剂选自二月桂酸二丁基锡和二(十二烷硫基)二丁基锡中的一种或多种。
- 根据权利要求1～5任一所述的热固型耐候保护涂层材料，其中，所述阻聚剂为酮类酸性有机溶剂。
- 根据权利要求1～6任一所述的热固型耐候保护涂层材料，所述阻聚剂选自乙酰丙酮、2-酮丁酸和丙酮酸中的一种或多种。
- 根据权利要求1～7任一所述的热固型耐候保护涂层材料，其中，所述表面活性剂包含改性有机硅类和丙烯酸酯类流平剂中的一种或多种。
- 根据权利要求8所述的热固型耐候保护涂层材料，所述改性有机硅类流平剂选自BYK333和BYK3550中的一种或多种。
- 根据权利要求8～9任一所述的热固型耐候保护涂层材料，所述丙烯酸酯类流平剂选自BYK3560和BYK3565中的一种或多种。
- 根据权利要求1～10任一所述的热固型耐候保护涂层材料，其中，所述有机溶剂选自乳酸乙酯、乙酸丁酯、乙酸乙酯和丙酸乙酯中的一种或多种。
- 根据权利要求1～11任一所述的热固型耐候保护涂层材料，其中，所述异氰酸酯类固化剂选自甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)、二苯基甲烷二异氰酸酯(MDI)、二环己基甲烷二异氰酸酯(HMDI)、六亚甲基二异氰酸酯(HDI)和赖氨酸二异氰酸酯(LDI)中的一种或多种。
- 一种用于制备根据权利要求1～12中任一项所述的热固型耐候保护涂层材料的方法，其包括：将预定比例的丙烯酸树脂、催化剂、阻聚剂、表面活性剂和有机溶剂混合以得到所述第一组分，并且称取预定比例的异氰酸酯类固化剂作为所述第二组分，以得到所述热固型耐候保护涂层材料。
- 根据权利要求1～12中任一项所述的热固型耐候保护涂层材料用于金属网格触控传感器的用途。
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| CN114933845A (zh) * | 2022-05-07 | 2022-08-23 | 浙江鑫柔科技有限公司 | 一种热固型耐候保护涂层材料及其制备方法和用途 |
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