CN113462232A - Water-proof antifouling photocureable coating and preparation method and application thereof - Google Patents
Water-proof antifouling photocureable coating and preparation method and application thereof Download PDFInfo
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- CN113462232A CN113462232A CN202110753726.2A CN202110753726A CN113462232A CN 113462232 A CN113462232 A CN 113462232A CN 202110753726 A CN202110753726 A CN 202110753726A CN 113462232 A CN113462232 A CN 113462232A
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- 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
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
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- 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
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
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Abstract
The invention relates to a water-resisting antifouling photocureable coating and a preparation method and application thereof. The waterproof antifouling photocureable coating comprises the following components in parts by weight: 5-20 parts of organic-inorganic hybrid resin, 5-15 parts of anti-fouling UV resin, 3-10 parts of photoinitiator, 45-75 parts of photocuring monomer, 0.1-5 parts of UV reaction type anti-fouling auxiliary agent, 0.1-5 parts of flatting agent and 0.1-5 parts of defoaming agent; the organic-inorganic hybrid resin is epoxy acrylate-silicon dioxide hybrid resin. The waterproof antifouling photocureable coating is suitable for surface treatment of LED display screens, the adhesion of the coating can reach the optimal 0 level, and the antifouling performance is excellent. The LED display screen subjected to the waterproof and antifouling surface treatment has more excellent cold and hot impact resistance and high temperature and high humidity resistance, meets the application requirements of the LED display screen indoors and outdoors, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of printing ink for LED display screens, and particularly relates to a waterproof antifouling photocureable coating as well as a preparation method and application thereof.
Background
An LED (semiconductor light emitting diode) display screen is a flat panel display, which is composed of small LED module panels, and is used for displaying various information such as characters, images, videos, and the like. The main light-emitting device of the LED display screen is a light-emitting chip, in order to prevent the light-emitting chip from losing efficacy due to water vapor corrosion or mechanical damage after being exposed in the air for a long time, the stability of the light-emitting chip is improved, surface packaging treatment is usually performed, most of the used packaging glue is epoxy resin glue, although a certain protection effect can be achieved, a large amount of hydroxyl groups are still remained on a branched chain after the epoxy resin is cured, the water absorption rate of a packaging glue layer is high, in long-term use, particularly in a high-temperature and high-humidity environment, water vapor in the air gradually permeates into the packaging glue layer to corrode the chip, and abnormal conditions such as short circuit, lamp death and the like are easily caused. In addition, the LED screen can leave fingerprints when touched by hands in the long-term use process, or is stained with dirt in the use environment, so that the video appearance and the appearance attractiveness are influenced. Consequently, carry out surperficial water proof antifouling treatment to the encapsulation glue film of LED screen, can not only improve the practicality of LED screen, prevent to become invalid, can improve its appearance quality moreover, promote user experience and feel.
In the prior art, a hydrophobic coating is usually coated on the surface of an LED display screen to obtain an antifouling coating, fluorine-containing or silicon-containing polymers are added into the coating, and fluorine-containing end groups cannot be fixed on the surface of the coating in a curing reaction, so that water-insulating and antifouling capacity in an ultrathin coating is insufficient, and the requirements of an LED screen on the adhesive force, heat resistance and moisture resistance of the LED screen cannot be met at the same time. Meanwhile, in order to improve the hardness of the coating and improve the wear resistance of the coating, the prior art adds inorganic filler particles into the formula, but the method causes the reduction of the light transmittance of the coating due to the compatibility problem of the inorganic particles and the UV light-cured resin, the monomer and the solvent. The patent CN112876955A discloses a fluorine-containing polyarylether-based super-hydrophobic coating with a scale-like shape and a preparation method thereof, wherein the preparation method comprises the steps of preparing fluorine-containing polyarylether by polycondensation of decafluorobiphenyl and hexafluorobisphenol A, dissolving the fluorine-containing polyarylether in a polar aprotic solvent, and adding a proper amount of SiO2Nano microsphere and carbon nanotube to obtain the paint. This patent utilizes the coarse structure of the micro-nano scale of scale form to improve water contact angle, but its fluorine-containing group can't be fixed in the coating surface, and the adhesive force on the substrate surface is not good.
Therefore, the development of the photocureable coating which has strong adhesive force, excellent heat and humidity resistance and water and dirt resistance and is used for the surface treatment of the LED display screen has important research significance and economic value.
Disclosure of Invention
Aiming at the problems that the prior art hydrophobic coating has poor adhesive force, poor waterproof and antifouling effects and can not realize heat and moisture resistance simultaneously, the invention provides a waterproof and antifouling photocureable coating. The waterproof antifouling photocureable coating takes epoxy acrylate-silicon dioxide hybrid resin as main resin, has the advantages of organic materials and inorganic materials, and is excellent in heat resistance and adhesiveness; the UV resin and the UV reaction type antifouling auxiliary agent are matched in a synergistic manner, so that the UV resin has excellent waterproof and antifouling performances, and the prepared photocuring coating has strong adhesive force and excellent heat resistance, and meets the requirements of cold and hot impact, temperature resistance and humidity resistance of an LED display screen.
The invention also aims to provide a preparation method of the water-resisting antifouling photocureable coating.
The invention also aims to provide application of the water-resistant antifouling photocureable coating in surface treatment of the LED display screen.
In order to achieve the purpose, the invention adopts the following technical scheme:
a waterproof antifouling photocureable coating comprises the following components in parts by weight:
the organic-inorganic hybrid resin is epoxy acrylate-silicon dioxide hybrid resin.
Because the surface of the LED display screen base material is an epoxy resin packaging adhesive layer, the epoxy acrylate is used as the main body resin, so that the epoxy acrylate has good compatibility with the packaging layer, and after the epoxy acrylate is specially hybridized with the nano silicon dioxide, the C-C molecular chain with smaller bond energy in the polymer is grafted with the Si-O bond with large bond energy, so that the thermal stability is stronger, the heat resistance, the hardness, the wear resistance and other properties of the epoxy acrylate are enhanced, the hybrid resin has the advantages of organic materials and inorganic materials, and the heat resistance and the adhesion are excellent; further, a coating formed by the photocuring coating can be firmly attached to the surface of the LED display screen, and the LED display screen is adaptive to the cold and hot impact requirements of the LED display screen and has excellent durability and weather resistance. And the diameter of the nano silicon dioxide is very small, so that the appearance of the hybrid resin is colorless and transparent, and the light emitting of the LED lamp is not influenced. And the diameter of the nano silicon dioxide is very small, so the particle size of the hybrid resin is small, the viscosity is low, the hybrid resin is suitable for preparing ink-jet printing coatings, and the resin has transparent appearance and does not influence the light emission of an LED lamp.
In addition, only the anti-fouling UV resin is adopted, so that the water-separating anti-fouling capability in the ultrathin coating is insufficient, and the requirements of an LED screen on the adhesive force, the heat resistance and the moisture resistance of the LED screen cannot be met at the same time generally; when the UV reactive antifouling auxiliary agent is used together, the UV reactive antifouling auxiliary agent and the UV reactive antifouling auxiliary agent have synergistic effect, so that a coating formed by the photocuring coating has excellent hydrophobic antifouling capacity, the coating further helps an LED display screen to isolate moisture on the basis of an encapsulation adhesive layer, and the inner lamp beads are protected from corrosion or short circuit.
Preferably, the water-resisting antifouling photocureable coating comprises the following components in parts by weight:
preferably, the molecular weight of the epoxy acrylate-silica hybrid resin is 1000-3000, and the structural formula is as follows:
preferably, the anti-fouling UV resin is one of fluorocarbon modified high-functionality polyurethane acrylate or fluorine-silicon modified high-functionality polyurethane acrylate.
It should be noted that when the functionality is greater than 4, it may be referred to as high functionality.
Preferably, the functionality of the anti-fouling UV resin is more than or equal to 8.
The high functionality can endow the anti-fouling UV resin with good hardness, so that the coating has the characteristics of wear resistance and scratch resistance.
Preferably, the photoinitiator is one or more of photoinitiator 907, photoinitiator ITX, photoinitiator 369, photoinitiator 784 and photoinitiator TPO.
Preferably, the light-curing monomer is one or more of a monofunctional monomer, a difunctional monomer or a trifunctional monomer.
Further preferably, the monofunctional monomer is one or more of cyclohexyl methacrylate, isobornyl acrylate, acryloyl morpholine, ethoxy ethyl acrylate and dicyclopentanyl methacrylate.
Further preferably, the bifunctional monomer is one or more of 1, 6-hexanediol diacrylate, tripropylene glycol diacrylate, neopentyl glycol diacrylate and tricyclodecane dimethanol diacrylate.
Further preferably, the trifunctional monomer is one or more of ethoxylated trimethylolpropane triacrylate, pentaerythritol triacrylate and pentaerythritol tetraacrylate.
Preferably, the UV reactive antifouling auxiliary agent is a terminal fluorine-containing acrylate.
Because the two ends of the end group fluorine-containing acrylate are respectively provided with the UV reactive group and the fluorine-containing group, after the internal UV curing reaction occurs, the fluorine-containing end group at the other end is fixed on the surface of the coating, and the fluorine concentration on the surface of the coating is greatly improved, thereby obtaining excellent waterproof and antifouling performances.
Preferably, the terminal fluorine-containing acrylate is one or more of perfluoroalkyl ethyl acrylate, methyl 2- (trifluoromethyl) acrylate, trifluoroethyl methacrylate, pentafluoropropyl acrylate, pentafluoropropyl methacrylate, octafluoropentyl methacrylate, heptadecafluorononyl methacrylate and heptadecafluorodecyl methacrylate.
Preferably, the leveling agent is one or more of BYK-UV3505, BYK-UV3510, BYK-UV3570, TEGO Glide 410, 432 or 450.
Preferably, the defoaming agent is one or more of BYK-1790, BYK-1794 and TEGO Airex 900 and 962.
The invention also provides a preparation method of the waterproof antifouling photocureable coating, which comprises the following steps:
uniformly mixing a photocuring monomer, a photoinitiator, organic-inorganic hybrid resin, anti-fouling UV resin, a flatting agent, a defoaming agent and a UV reaction type anti-fouling auxiliary agent, and filtering to obtain the waterproof and anti-fouling photocuring coating.
Further preferably, the preparation method of the water-resistant antifouling photocureable coating comprises the following steps:
s1, uniformly mixing all the photo-curing monomers, and adding the photoinitiator into the photo-curing monomer mixed solution for full dissolution;
s2, adding organic-inorganic hybrid resin and anti-fouling UV resin into the mixed solution obtained in the step S1, and uniformly mixing to form mixed solution;
s3, adding a leveling agent and a defoaming agent into the mixed solution obtained in the step S2, and uniformly mixing to form a mixed solution;
and S4, adding the UV reaction type antifouling auxiliary agent into the mixed solution obtained in the step S3 while stirring, uniformly mixing, and filtering through a 1-micron filter membrane to obtain the waterproof antifouling photocureable coating.
The application of the water-proof antifouling photocureable coating in the surface treatment of the LED display screen is also within the protection scope of the invention.
In the application of the waterproof antifouling photocureable coating in the surface treatment of the LED display screen, the following modes are adopted:
and (2) filling the photocuring coating into an ink-jet printer, spray-printing the photocuring coating on the LED display module, carrying out ultraviolet curing to obtain the LED display module subjected to water-proof and antifouling treatment, and then forming a complete LED display screen in a module splicing mode.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention provides a waterproof antifouling photocureable coating, which takes epoxy acrylate-silicon dioxide hybrid resin as main resin, can be tightly combined with an epoxy resin packaging adhesive layer, has strong adhesive force and excellent heat resistance, and meets the requirements of cold and hot impact, temperature resistance and humidity resistance of an LED display screen.
(2) The water-proof antifouling photocureable coating adopts the synergy of the antifouling UV resin and the UV reaction type antifouling auxiliary agent, enhances the concentration of fluorine-containing hydrophobic groups on the surface of the coating, enables the LED display screen to have excellent waterproof and fingerprint-proof dirt adhesion functions after the surface treatment of the coating, and keeps clean in long-term use.
(3) The waterproof antifouling photocureable coating provided by the invention is low in viscosity, small in particle size, free of solid particles, very suitable for inkjet printing, simple and efficient in process and suitable for being applied to surface treatment of an LED display screen by matching with an ultraviolet curing process.
Detailed Description
The invention is further illustrated by the following examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Experimental procedures without specific conditions noted in the examples below, generally according to conditions conventional in the art or as suggested by the manufacturer; the raw materials, reagents and the like used are, unless otherwise specified, those commercially available from the conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
The performance test methods and standards for the coatings of the examples and comparative examples of the present invention are as follows:
(1) adhesion force: the tests were carried out according to the test of the grid drawing of GB/T9286-1998 paint and varnish films
(2) And (3) anti-fouling test: and (4) scratching the surface of the waterproof antifouling coating of the LED display screen by using an oily pen, and observing a penetration result and a wiping result.
(3) Contact angle: and (3) dripping water on the surface of the waterproof antifouling coating of the LED display screen by using a contact angle tester, and measuring the contact angle of the water to the coating.
(4) And (3) testing cold and hot impact: and (3) placing the LED display screen with the surface sprayed and printed with the water-proof and antifouling coating and cured into a cold and hot impact test box, circulating for 200 times at-40 ℃ (15min) and 100 ℃ (15min), and observing whether the surface has cracks or not.
(5) High temperature and high humidity test: and (3) placing the LED display screen with the surface sprayed and printed with the cured waterproof antifouling coating into a constant-temperature constant-humidity test box, placing the LED display screen for 1000 hours under the conditions of 80 ℃ of temperature and 90 parts of humidity, and observing whether a lamp is dead or not.
Example 1
The embodiment provides a waterproof antifouling photocureable coating which comprises the following components in parts by weight:
the preparation method of the photocureable coating for water resistance and antifouling comprises the following steps:
s1, uniformly mixing ethoxy ethyl acrylate, 1, 6-hexanediol diacrylate and pentaerythritol triacrylate, and adding photoinitiators TPO and 369 into the photocuring monomer mixed solution for full dissolution;
s2, adding epoxy acrylate-silicon dioxide hybrid resin and fluorocarbon modified octafunctional polyurethane acrylate into the mixed solution obtained in the step S1, and uniformly mixing to form a mixed solution;
s3, adding BYK-UV3505 and BYK-1794 into the mixed solution obtained in the step S2, and uniformly mixing to form a mixed solution;
and S4, adding perfluoroalkyl ethyl acrylate into the mixed liquid obtained in the step S3 while stirring, uniformly mixing, and filtering through a 1-micron filter membrane to obtain the photocuring coating for the water-proof and anti-fouling treatment of the surface of the LED display screen.
Example 2
The embodiment provides a waterproof antifouling photocureable coating which comprises the following components in parts by weight:
the preparation method of the waterproof antifouling photocureable coating specifically comprises the following steps:
s1, uniformly mixing acryloyl morpholine, neopentyl glycol diacrylate and trimethylolpropane triacrylate, and adding photoinitiators TPO, 907 and ITX into the photocuring monomer mixed solution for full dissolution;
s2, adding epoxy acrylate-silicon dioxide hybrid resin and fluorine-silicon modified nine-functional polyurethane acrylate into the mixed solution obtained in the step S1, and uniformly mixing to form a mixed solution;
s3, adding BYK-UV3570 and BYK-1790 into the mixed solution obtained in the step S2, and uniformly mixing to form a mixed solution;
and S4, adding heptadecafluorodecyl methacrylate into the mixed solution obtained in the step S3 while stirring, uniformly mixing, and filtering through a filter membrane of 1 micron to obtain the photocuring coating for the water-resisting and anti-fouling treatment of the surface of the LED display screen.
Example 3
The embodiment provides a waterproof antifouling photocureable coating which comprises the following components in parts by weight:
the preparation method of the waterproof antifouling photocureable coating specifically comprises the following steps:
s1, uniformly mixing cyclohexyl methacrylate, tripropylene glycol diacrylate and ethoxylated trimethylolpropane triacrylate, and adding photoinitiators ITX and 369 into the photocuring monomer mixed solution for full dissolution;
s2, adding epoxy acrylate-silicon dioxide hybrid resin and fluorosilicone modified octafunctional polyurethane acrylate into the mixed solution obtained in the step S1, and uniformly mixing to form a mixed solution;
s3, adding TEGO Glide 410 and TEGO Airex 900 into the mixed solution obtained in the step S2, and uniformly mixing to form a mixed solution;
and S4, adding 2- (trifluoromethyl) methyl acrylate into the mixed solution obtained in the step S3 while stirring, uniformly mixing, and filtering through a 1-micron filter membrane to obtain the photocuring paint for the water-proof and anti-fouling treatment of the surface of the LED display screen.
Comparative example 1
This comparative example is used to compare with example 1 and to investigate the effect of the epoxy acrylate-silica hybrid resin of the present invention on the overall performance of the coating. The comparative example specifically includes the following components in mass fraction:
the preparation procedure was the same as in example 1.
Comparative example 2
This comparative example was used to study the effect of the UV reactive antifouling auxiliary of the present invention on the overall performance of the photocurable coating, in comparison with example 1. The comparative example specifically includes the following components in mass fraction:
the preparation procedure was the same as in example 1.
Performance characterization
The water-resistant antifouling photocuring coating prepared in the embodiment is filled into an ink-jet printer, is jet-printed on an LED display module to obtain an ultrathin coating, is subjected to ultraviolet curing for 10 seconds to obtain an LED display module subjected to water-resistant antifouling surface treatment, then forms a complete LED display screen in a module splicing mode, and is subjected to performance test on a coating sample, and the results are shown in table 1.
TABLE 1 Properties of Water-and soil-repellent photocured coatings in examples and comparative examples
As can be seen from the table above, the ultra-thin coatings of the waterproof and antifouling coatings of examples 1 to 3 have excellent adhesion, which all reach 0 grade, and simultaneously have excellent antifouling performance, a water contact angle of more than 150 degrees and super-hydrophobic performance. The LED display screen subjected to the waterproof and antifouling surface treatment has more excellent cold and heat shock resistance and high temperature and humidity resistance, does not crack after being cycled for 200 times from-40 ℃ (15min) to 100 ℃ (15min), does not have dead lamps after 80 ℃/90 parts of R.H.1000 hours, and meets the application requirements of the LED display screen indoors and outdoors.
The coating of comparative example 1, which does not contain epoxy acrylate-silica hybrid resin, has a reduced adhesion to the encapsulating adhesive layer of grade 3, insufficient heat resistance, surface cracking after a cold and heat shock test, and a small amount of dead lamps after a high temperature and high humidity test; the coating of comparative example 2, which does not contain the UV reactive antifouling assistant, has reduced water barrier properties and antifouling properties, and a water contact angle of less than 150 °. In conclusion, the photocuring coating prepared by the specific formula has excellent comprehensive performance, is suitable for water-resisting and antifouling treatment of the surface of the LED display screen, and has wide application prospect.
The principles and embodiments of the present invention have been described herein using specific examples, which are provided only to help understand the method and the core concept of the present invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, the specific embodiments and the application range may be changed. In view of the above, the present disclosure should not be construed as limiting the invention.
Claims (10)
1. The waterproof antifouling photocureable coating is characterized by comprising the following components in parts by weight:
the organic-inorganic hybrid resin is epoxy acrylate-silicon dioxide hybrid resin.
2. The water-resistant antifouling photocurable coating as claimed in claim 1, wherein the molecular weight of the epoxy acrylate-silica hybrid resin is 1000-3000, and the structural formula thereof is as follows:
3. the water-resistant antifouling photocurable coating according to claim 1, wherein the antifouling UV resin is one of fluorocarbon-modified high-functionality polyurethane acrylate or fluorosilicone-modified high-functionality polyurethane acrylate; the functionality of the anti-fouling UV resin is more than or equal to 8.
4. The water-resistant antifouling photocurable coating as claimed in claim 1, wherein the photoinitiator is one or more of photoinitiator 907, photoinitiator ITX, photoinitiator 369, photoinitiator 784 or photoinitiator TPO.
5. The water-resistant antifouling photocurable coating according to claim 1, wherein the photocurable monomer is one or more of a monofunctional monomer, a difunctional monomer or a trifunctional monomer.
6. The water-resistant antifouling photocurable coating according to claim 1, wherein the UV-reactive antifouling auxiliary is a terminal fluoroacrylate.
7. The water-resistant antifouling photocurable coating according to claim 6, wherein the terminal fluoroacrylate is one or more of perfluoroalkylethyl acrylate, methyl 2- (trifluoromethyl) acrylate, trifluoroethyl methacrylate, pentafluoropropyl acrylate, pentafluoropropyl methacrylate, octafluoropentyl methacrylate, heptadecafluorononyl methacrylate, or heptadecafluorodecyl methacrylate.
8. The water-resistant antifouling photocureable coating of claim 1, wherein the leveling agent is one or more of BYK-UV3505, BYK-UV3510, BYK-UV3570, TEGO Glide 410, 432 or 450; the defoaming agent is one or more of BYK-1790, BYK-1794 and TEGO Airex 900 and 962.
9. The preparation method of the water-resisting antifouling photocureable coating is characterized by comprising the following steps: uniformly mixing a photocuring monomer, a photoinitiator, organic-inorganic hybrid resin, anti-fouling UV resin, a flatting agent, a defoaming agent and a UV reaction type anti-fouling auxiliary agent, and filtering to obtain the waterproof and anti-fouling photocuring coating.
10. The application of the water-resisting antifouling photocureable coating of any one of claims 1 to 8 in surface treatment of LED display screens.
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Application publication date: 20211001 |