Color LED-UV glass coating and preparation method thereof
By introducing rigid hydrophilic monomers and ultraviolet absorbing functional groups into the acrylate coating, the problem of insufficient hardness and anti-ultraviolet aging performance of the coating is solved, and the effects of high hardness, flexibility and anti-ultraviolet aging are achieved.
Patent Information
- Application Number
- CN202410073120.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-01-18
- Publication Date
- 2025-08-29
- Estimated Expiration
- 2044-01-18
AI Technical Summary
The existing acrylate coatings have insufficient flexibility and hardness, and have poor anti-ultraviolet aging performance.
Rigid hydrophilic monomer and crosslinking agent containing ultraviolet absorbing functional groups in the structure are prepared by amine esterification reaction, and added to the acrylate prepolymer to form a coating with sulfonic acid groups and polyether derivatives, which improves the hardness and resistance to UV aging.
It improves the hardness and flexibility of the paint, and also has good anti-UV aging properties, avoiding the paint from yellowing after multiple UV irradiation.
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Figure CN117903653B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of coatings, and in particular to a colored LED-UV glass coating and a preparation method thereof. Background Art
[0002] UV coating, or ultraviolet light-curing coating, is a type of coating that can generate free radicals under ultraviolet light, further undergo polymerization reactions, and gradually solidify into a film. Traditional UV coatings mainly use mercury lamps as light sources, which have high energy consumption, short service life, and produce ozone, which is not conducive to environmental protection. LED-UV coatings are a type of light-curing coatings. LED-UV is a low-energy curing light source that emits a single-wavelength ultraviolet light source, mainly 365nm and 395nm. It can be used as a radiation source to achieve the curing of UV coatings. It is environmentally friendly, highly safe, and has low energy consumption. Therefore, LED-UV coatings have more significant advantages and broad market prospects.
[0003] With growing awareness of environmental protection and energy conservation, coupled with the continuous advancement of related technologies, the market prospects for colored LED-UV glass coatings are promising. These coatings are widely used in architecture, furniture, automotive, and other fields, becoming an important decorative and functional material. Furthermore, with decreasing production costs and improved application technology, the market share of LED-UV glass coatings is expected to further expand.
[0004] In order for the coating to effectively protect the glass, the prepared coating should have good flexibility and hardness, as well as good adhesion. Although common acrylic coatings have good weather resistance and corrosion resistance, their flexibility and hardness are slightly insufficient. In addition, since LED-UV light sources generally require multiple reciprocating irradiations, the coating needs to have good UV resistance to avoid yellowing and negative effects.
[0005] To this end, the present invention provides an LED-UV glass coating that can exhibit good strength and flexibility and has good resistance to ultraviolet aging. Summary of the Invention
[0006] (1) Technical problems solved
[0007] In view of the shortcomings of the existing technology, the present invention provides a colored LED-UV glass coating and a preparation method thereof, which solves the problems of insufficient flexibility and hardness and poor anti-ultraviolet aging performance of acrylic coatings.
[0008] (2) Technical solution
[0009] A colored LED-UV glass coating comprises the following raw materials, calculated by weight: 10-20 parts of methyl methacrylate, 10-20 parts of isobutyl acrylate, 5-10 parts of butyl acrylate, 5-10 parts of hydroxyethyl methacrylate, 2-4 parts of a rigid hydrophilic monomer, 1-3 parts of a crosslinking agent, 0.1-0.2 parts of an initiator, 2-3 parts of an LED photoinitiator, 0.5-1.5 parts of a defoaming agent, 0.5-1.5 parts of a leveling agent, 8-12 parts of a pigment, and 25-40 parts of purified water;
[0010] The rigid hydrophilic monomer is prepared from 3-isopropyl-dimethylbenzyl isocyanate and N-hydroxysuccinimide sulfonic acid sodium salt as raw materials;
[0011] The cross-linking agent is a polyether derivative containing an ultraviolet absorption functional group in its structure.
[0012] Further preferably, the preparation method of the rigid hydrophilic monomer is as follows:
[0013] 3-isopropyl-dimethylbenzyl isocyanate, sodium salt of N-hydroxysuccinimide sulfonic acid, and toluene are added sequentially to a reaction flask filled with nitrogen. Stirring is started. After a homogeneous solution is formed, the heating process is started and the temperature is raised to 70-80°C. The tin catalyst is then added to the flask. After complete addition, the solution is kept warm for 2-4 hours under continuous stirring. The solvent and low-boiling substances are evaporated. After purification, the product can be obtained to obtain a rigid hydrophilic monomer. The structural formula of 3-isopropyl-dimethylbenzyl isocyanate is:
[0014]
[0015] N-Hydroxysuccinimide Sulfonic Acid Sodium Salt Structural Formula:
[0016]
[0017] In the above technical solution, 3-isopropyl-dimethylbenzyl isocyanate and sodium salt of N-hydroxysuccinimide sulfonic acid are used as raw materials, toluene is used as solvent, and the catalytic effect of a tin catalyst is utilized to promote an amine esterification reaction between the isocyanate group and the hydroxyl group of the raw materials to prepare a rigid hydrophilic monomer containing a sulfonic acid succinimide group and an unsaturated alkenyl functional group in the structure. The structural formula of the rigid hydrophilic monomer is shown in the figure below:
[0018]
[0019] More preferably, the molar ratio of the 3-isopropyl-dimethylbenzyl isocyanate to the sodium salt of N-hydroxysuccinimide sulfonate is 1:1-1.2.
[0020] More preferably, the tin catalyst is at least one of dibutyltin didodecylsulfide, stannous octoate, dibutyltin dilaurate or dibutyltin diacetate.
[0021] Further preferably, the preparation method of the cross-linking agent is as follows:
[0022] Add the epoxy-terminated allyl polyether and acetonitrile to a reaction flask, mix them mechanically until uniform, introduce nitrogen, expel the air in the flask, turn on the heating, and when the temperature is maintained at 60-70°C, add 2,2',4,4'-tetrahydroxybenzophenone and the catalyst under continuous stirring. Stir well after addition, keep warm and stir for 6-8 hours, evaporate to remove low-boiling substances and solvent, separate the product, and vacuum dry it to obtain the cross-linking agent.
[0023] Epoxy-terminated allyl polyether structural formula (n is an integer less than 20)
[0024]
[0025] 2,2',4,4'-Tetrahydroxybenzophenone structure
[0026]
[0027] In the above technical solution, acetonitrile is used as a solvent, an epoxy-terminated allyl polyether and 2,2',4,4'-tetrahydroxybenzophenone are used as reactants, and a catalyst is used to catalyze the ring-opening addition of the epoxy group in the epoxy-terminated allyl polyether structure with the para-hydroxyl group in the 2,2',4,4'-tetrahydroxybenzophenone structure. By controlling the molar ratio of the reactants to make the 2,2',4,4'-tetrahydroxybenzophenone excessive, a polyether derivative containing a benzophenone ultraviolet absorption functional group and two equivalents of unsaturated alkenyl functional groups in its structure can be prepared.
[0028] More preferably, the average molecular weight of the epoxy-terminated allyl polyether is 450-1000.
[0029] More preferably, the molar ratio of the epoxy-terminated allyl polyether to 2,2',4,4'-tetrahydroxybenzophenone is 1:2-2.5.
[0030] Further preferably, the catalyst is boron trifluoride etherate complex, and the added amount of the catalyst is 1-3% of the total mass of the epoxy-terminated allyl polyether and 2,2',4,4'-tetrahydroxybenzophenone.
[0031] Further preferably, the initiator is benzoyl peroxide or dicumyl peroxide; the LED photoinitiator is at least one of photoinitiator 819, photoinitiator 907 or photoinitiator 369; the defoamer is BYK-1790 non-silicone defoamer; the leveling agent is an acrylate leveling agent; and the pigment is at least one of carbon black, iron red and Prussian blue.
[0032] A method for preparing a colored LED-UV glass coating comprises the following steps:
[0033] Step 1: Preparation of acrylate prepolymer
[0034] Add half part by weight of methyl methacrylate, isobutyl acrylate, butyl acrylate, hydroxyethyl methacrylate and rigid hydrophilic monomer to purified water, stir and mix evenly, heat to 60-70°C, keep stirring for 2-4 hours, add the remaining amount of methyl methacrylate, isobutyl acrylate, butyl acrylate and hydroxyethyl methacrylate, and continue to add crosslinking agent and initiator, keep warm for 4-6 hours to form acrylate prepolymer;
[0035] Step 2: Prepare glass coating
[0036] Add leveling agent and pigment to acrylate prepolymer, stir and mix at a stirring rate of 800-1000 r / min for 20-30 minutes, add LED photoinitiator and defoamer, adjust the stirring rate to 300-500 r / min, and continue stirring for 5-10 minutes to prepare glass coating.
[0037] (3) Beneficial technical effects
[0038] a) The present invention prepares a rigid hydrophilic monomer and participates in the polymerization process of the glass coating, thereby introducing a highly polar sulfonic acid hydrophilic functional group and a rigid succinimide ring into the acrylate molecular chain. Utilizing the strong hydrophilic effect of the sulfonic acid group, the glass coating exhibits the properties of a water-based coating, avoiding the generation of volatiles and the problem of environmental pollution. In addition, the presence of the rigid succinimide heterocycle can improve the hardness of the coating.
[0039] b) The present invention uses a polyether derivative containing a UV-absorbing functional group as a crosslinking agent. On the one hand, the polyether structure contains a large number of ether bonds, and the polyether molecular chain is highly flexible, which can improve the adhesion and flexibility of the coating. At the same time, after crosslinking, the crosslinking density of the acrylate molecular chain is higher, which can have a higher cohesive force, thereby further enhancing the adhesion of the coating. On the other hand, the benzophenone UV-absorbing functional group contained in the crosslinking agent can prevent the coating from yellowing after repeated UV exposure, giving the coating good resistance to UV aging. BRIEF DESCRIPTION OF THE DRAWINGS
[0040] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying any creative work.
[0041] Figure 1 This is the infrared analysis spectrum of the rigid hydrophilic monomer;
[0042] Figure 2 This is the infrared analysis spectrum of the cross-linking agent. DETAILED DESCRIPTION
[0043] To facilitate understanding of the present invention, the present invention will be described in more detail below. Preferred embodiments of the present invention are provided below. However, the present invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a more thorough and comprehensive understanding of the disclosure of the present invention.
[0044] The rigid hydrophilic monomers used in the following examples and comparative examples were prepared by the following method:
[0045] To a reaction bottle filled with nitrogen, 1.2 g of 3-isopropyl-dimethylbenzyl isocyanate, 1.4 g of N-hydroxysuccinimide sulfonic acid sodium salt and toluene were added in sequence, stirring was started, and after a homogeneous solution was formed, the heating program was started and the temperature was raised to 75°C. Then 0.1 g of stannous octoate was added to the bottle. After the addition was complete, the solution was kept warm for 3 hours under constant stirring, and the solvent and low-boiling substances were evaporated. After purification, the product was obtained to obtain a rigid hydrophilic monomer.
[0046] The rigid hydrophilic monomer was analyzed and tested using a Brucker Tensor 27 Fourier transform infrared spectrometer. The results are as follows: Figure 1 As shown, the analysis shows that 3402cm -1 The characteristic stretching vibration absorption peak of -OH in sulfonic acid appears at 3087cm -1 and 3056cm -1 The characteristic stretching vibration peak of carbon and hydrogen belonging to the benzene ring appeared at 3010cm -1 The carbon-hydrogen stretching vibration absorption peak attributed to the carbon-carbon double bond appeared at 1748 cm -1 The characteristic stretching vibration peak of C=O in the amine ester bond appeared at 1667cm -1 The characteristic stretching vibration absorption peak of C=O in succinimide appeared at 1319 cm -1 A S=O asymmetric stretching vibration peak attributed to sulfonic acid appeared at .
[0047] The cross-linking agents used in the following examples and comparative examples were prepared by the following method:
[0048] 1.8 g of epoxy-terminated allyl polyether with an average molecular weight of 1000 and acetonitrile were added to a reaction flask. After mechanical mixing, nitrogen was introduced to expel the air in the flask, and heating was turned on. When the temperature was maintained at 65°C, 1 g of 2,2',4,4'-tetrahydroxybenzophenone and 0.05 g of boron trifluoride ether complex were added under continuous stirring. After the addition, the mixture was stirred evenly. After the reaction was stirred at this temperature for 8 hours, low-boiling substances and solvents were evaporated to remove the low-boiling substances and solvents, and the product was separated and dried in vacuo to obtain the cross-linking agent.
[0049] Figure 2 This is the infrared analysis test chart of the crosslinking agent. After analysis, 3391cm -1 The characteristic stretching vibration peak attributed to the hydroxyl group appeared at 3096 cm -1 and 3071cm -1 The carbon-hydrogen stretching vibration peak attributed to the benzene ring appeared at 3036 cm -1 The carbon-hydrogen stretching vibration peak attributed to the unsaturated olefin group appeared at 1715 cm -1 The C=O stretching vibration absorption peak at 1087 cm-1, which is attributed to the benzophenone group, appears at -1 A characteristic absorption peak attributed to the ether bond appeared at
[0050] Example 1
[0051] A colored LED-UV glass coating comprises the following raw materials, calculated by weight: 10 parts of methyl methacrylate, 10 parts of isobutyl acrylate, 5 parts of butyl acrylate, 5 parts of hydroxyethyl methacrylate, 2 parts of a rigid hydrophilic monomer, 1 part of a crosslinking agent, 0.1 parts of benzoyl peroxide, 8192 parts of an LED photoinitiator, 0.5 parts of a defoaming agent BYK-1790, 0.5 parts of an EFKA FL 3600 acrylic wetting and leveling agent, 8 parts of an iron oxide red pigment, and 25 parts of purified water.
[0052] The preparation method of the coating comprises the following steps:
[0053] Step 1: Preparation of acrylate prepolymer
[0054] Add one-half part by weight of methyl methacrylate, isobutyl acrylate, butyl acrylate, hydroxyethyl methacrylate and a rigid hydrophilic monomer to purified water, stir and mix evenly, heat to 60°C, keep stirring for 2 hours, add the remaining amount of methyl methacrylate, isobutyl acrylate, butyl acrylate and hydroxyethyl methacrylate, and continue to add a crosslinking agent and benzoyl peroxide, keep warm for 4 hours to form an acrylate prepolymer;
[0055] Step 2: Prepare glass coating
[0056] EFKA FL 3600 acrylic wetting and leveling additive and iron red pigment were added to the acrylate prepolymer, and the mixture was stirred at a stirring rate of 800 r / min for 30 minutes. Then, LED photoinitiator 819 and defoamer BYK-1790 were added, and the stirring rate was adjusted to 300 r / min. The mixture was stirred for 10 minutes to prepare the glass coating.
[0057] Example 2
[0058] A colored LED-UV glass coating comprises the following raw materials, calculated by weight: 18 parts of methyl methacrylate, 15 parts of isobutyl acrylate, 6 parts of butyl acrylate, 8 parts of hydroxyethyl methacrylate, 3 parts of a rigid hydrophilic monomer, 2.5 parts of a crosslinking agent, 0.2 parts of benzoyl peroxide, 9073 parts of an LED photoinitiator, 1 part of a defoamer BYK-1790, 1 part of an EFKAFL 3600 acrylic wetting and leveling agent, 10 parts of a Prussian blue pigment, and 35 parts of purified water.
[0059] The preparation method of the coating comprises the following steps:
[0060] Step 1: Preparation of acrylate prepolymer
[0061] Add one-half part by weight of methyl methacrylate, isobutyl acrylate, butyl acrylate, hydroxyethyl methacrylate and a rigid hydrophilic monomer to purified water, stir and mix evenly, heat to 65°C, keep stirring for 3 hours, then add the remaining amount of methyl methacrylate, isobutyl acrylate, butyl acrylate and hydroxyethyl methacrylate, and continue to add a crosslinking agent and benzoyl peroxide, keep warm for 4 hours to form an acrylate prepolymer;
[0062] Step 2: Prepare glass coating
[0063] EFKA FL 3600 acrylic wetting and leveling additive and Prussian blue pigment were added to the acrylate prepolymer, and the mixture was stirred at a stirring rate of 1000 r / min for 20 minutes. Then, LED photoinitiator 907 and defoamer BYK-1790 were added, and the stirring rate was adjusted to 500 r / min. The mixture was stirred for 5 minutes to prepare the glass coating.
[0064] Example 3
[0065] A colored LED-UV glass coating comprises the following raw materials, calculated by weight: 20 parts of methyl methacrylate, 20 parts of isobutyl acrylate, 10 parts of butyl acrylate, 10 parts of hydroxyethyl methacrylate, 4 parts of a rigid hydrophilic monomer, 3 parts of a crosslinking agent, 0.2 parts of benzoyl peroxide, 3693 parts of an LED photoinitiator, 1.5 parts of a defoaming agent BYK-1790, 1.5 parts of an EFKAFL 3600 acrylic wetting and leveling agent, 12 parts of a Prussian blue pigment, and 40 parts of purified water.
[0066] The preparation method of the coating comprises the following steps:
[0067] Step 1: Preparation of acrylate prepolymer
[0068] Add one-half part by weight of methyl methacrylate, isobutyl acrylate, butyl acrylate, hydroxyethyl methacrylate and a rigid hydrophilic monomer to purified water, stir and mix evenly, heat to 70°C, keep stirring for 2 hours, add the remaining amount of methyl methacrylate, isobutyl acrylate, butyl acrylate and hydroxyethyl methacrylate, and continue to add a crosslinking agent and benzoyl peroxide, keep warm for 6 hours to form an acrylate prepolymer;
[0069] Step 2: Prepare glass coating
[0070] EFKA FL 3600 acrylic wetting and leveling additive and Prussian blue pigment were added to the acrylate prepolymer, and the mixture was stirred at a stirring rate of 1000 r / min for 20 minutes. Then, LED photoinitiator 369 and defoamer BYK-1790 were added, and the stirring rate was adjusted to 500 r / min. The mixture was stirred for 5 minutes to prepare the glass coating.
[0071] Comparative Example 1
[0072] A colored LED-UV glass coating, comprising the following raw materials, calculated by weight: 18 parts of methyl methacrylate, 15 parts of isobutyl acrylate, 6 parts of butyl acrylate, 8 parts of hydroxyethyl methacrylate, 2.5 parts of a crosslinking agent, 0.2 parts of benzoyl peroxide, 9073 parts of an LED photoinitiator, 1 part of a defoamer BYK-1790, 1 part of an EFKAFL 3600 acrylic wetting and leveling agent, 10 parts of a Prussian blue pigment, and 35 parts of purified water;
[0073] The preparation method of the coating comprises the following steps:
[0074] Step 1: Preparation of acrylate prepolymer
[0075] Add one-half part by weight of methyl methacrylate, isobutyl acrylate, butyl acrylate, and hydroxyethyl methacrylate to purified water, stir and mix evenly, then heat to 65°C, keep stirring for 3 hours, add the remaining amount of methyl methacrylate, isobutyl acrylate, butyl acrylate, and hydroxyethyl methacrylate, and continue to add a crosslinking agent and benzoyl peroxide, and keep warm for 4 hours to form an acrylate prepolymer;
[0076] Step 2: Prepare glass coating
[0077] EFKA FL 3600 acrylic wetting and leveling additive and Prussian blue pigment were added to the acrylate prepolymer, and the mixture was stirred at a stirring rate of 1000 r / min for 20 minutes. Then, LED photoinitiator 907 and defoamer BYK-1790 were added, and the stirring rate was adjusted to 500 r / min. The mixture was stirred for 5 minutes to prepare the glass coating.
[0078] Comparative Example 2
[0079] A colored LED-UV glass coating comprises the following raw materials, calculated by weight: 18 parts of methyl methacrylate, 15 parts of isobutyl acrylate, 6 parts of butyl acrylate, 8 parts of hydroxyethyl methacrylate, 3 parts of a rigid hydrophilic monomer, 0.2 parts of benzoyl peroxide, 9073 parts of an LED photoinitiator, 1 part of a defoamer BYK-1790, 1 part of an EFKAFL 3600 acrylic wetting and leveling agent, 10 parts of a Prussian blue pigment, and 35 parts of purified water.
[0080] The preparation method of the coating comprises the following steps:
[0081] Step 1: Preparation of acrylate prepolymer
[0082] Add one-half part by weight of methyl methacrylate, isobutyl acrylate, butyl acrylate, hydroxyethyl methacrylate and a rigid hydrophilic monomer to purified water, stir and mix evenly, heat to 65°C, keep stirring for 3 hours, then add the remaining amount of methyl methacrylate, isobutyl acrylate, butyl acrylate and hydroxyethyl methacrylate, and continue to add benzoyl peroxide, keep warm for 4 hours to form an acrylate prepolymer;
[0083] Step 2: Prepare glass coating
[0084] EFKA FL 3600 acrylic wetting and leveling additive and Prussian blue pigment were added to the acrylate prepolymer, and the mixture was stirred at a stirring rate of 1000 r / min for 20 minutes. Then, LED photoinitiator 907 and defoamer BYK-1790 were added, and the stirring rate was adjusted to 500 r / min. The mixture was stirred for 5 minutes to prepare the glass coating.
[0085] Comparative Example 3
[0086] A colored LED-UV glass coating, comprising the following raw materials, calculated by weight: 18 parts of methyl methacrylate, 15 parts of isobutyl acrylate, 6 parts of butyl acrylate, 8 parts of hydroxyethyl methacrylate, 0.2 parts of benzoyl peroxide, 9073 parts of an LED photoinitiator, 1 part of a defoamer BYK-1790, 1 part of an EFKAFL 3600 acrylic wetting and leveling agent, 10 parts of a Prussian blue pigment, and 35 parts of purified water;
[0087] The preparation method of the coating comprises the following steps:
[0088] Step 1: Preparation of acrylate prepolymer
[0089] Add one-half part by weight of methyl methacrylate, isobutyl acrylate, butyl acrylate, and hydroxyethyl methacrylate to purified water, stir and mix evenly, then heat to 65°C, keep stirring for 3 hours, add the remaining amount of methyl methacrylate, isobutyl acrylate, butyl acrylate, and hydroxyethyl methacrylate, and continue to add benzoyl peroxide, keep warm for 4 hours to form an acrylate prepolymer;
[0090] Step 2: Prepare glass coating
[0091] EFKA FL 3600 acrylic wetting and leveling additive and Prussian blue pigment were added to the acrylate prepolymer, and the mixture was stirred at a stirring rate of 1000 r / min for 20 minutes. Then, LED photoinitiator 907 and defoamer BYK-1790 were added, and the stirring rate was adjusted to 500 r / min. The mixture was stirred for 5 minutes to prepare the glass coating.
[0092] The coatings prepared in Examples 1 to 3 and Comparative Examples 1 to 3 were uniformly coated on the tinplate surface and UV-cured. The properties of the resulting coatings were tested, and the results are recorded in Table 1:
[0093] Table 1 - Performance test results
[0094]
[0095]
[0096] Note: Hardness is tested according to GB / T 6739-2006; flexibility is tested according to GB / T1731-2020; adhesion is tested according to GB / T 1720-2020; and UV resistance is tested according to GB / T 23983-2009.
[0097] Analysis of the data in the table shows that, compared to the coating prepared in Comparative Example 3 without the addition of a rigid hydrophilic monomer, the coatings prepared in Examples 1 to 3 of the present invention clearly exhibited good hardness, flexibility, adhesion, and UV aging resistance. The coating prepared in Comparative Example 1, in which no rigid hydrophilic monomer was added, showed a significant decrease in hardness, while other properties were good. The coating prepared in Comparative Example 2, in which no crosslinking agent was added, showed a significant decrease in flexibility, adhesion, and UV aging resistance, and a slight decrease in hardness. This is presumably due to the low crosslinking density of the coating formed by the uncrosslinked acrylate molecular chains, resulting in a relatively poor coating density, which resulted in a decrease in hardness.
[0098] Based on the ideal embodiments of the present invention, and with reference to the above description, relevant personnel can make various changes and modifications without departing from the technical scope of the present invention. The technical scope of the present invention is not limited to the contents of the specification, but must be determined according to the scope of the claims.
Claims
1. A colored LED-UV glass coating, characterized in that: The raw materials include the following in parts by weight: 10-20 parts of methyl methacrylate, 10-20 parts of isobutyl acrylate, 5-10 parts of butyl acrylate, 5-10 parts of hydroxyethyl methacrylate, 2-4 parts of rigid hydrophilic monomer, 1-3 parts of crosslinking agent, 0.1-0.2 parts of initiator, 2-3 parts of LED photoinitiator, 0.5-1.5 parts of defoaming agent, 0.5-1.5 parts of leveling agent, 8-12 parts of pigment, and 25-40 parts of purified water; The rigid hydrophilic monomer is prepared from 3-isopropyl-dimethylbenzyl isocyanate and N-hydroxysuccinimide sulfonic acid sodium salt as raw materials; The cross-linking agent is a polyether derivative containing an ultraviolet absorbing functional group in its structure; The preparation method of the cross-linking agent is as follows: Add the epoxy-terminated allyl polyether and acetonitrile to a reaction flask, mix them mechanically until uniform, introduce nitrogen, expel the air in the flask, turn on the heating, and when the temperature is maintained at 60-70°C, add 2,2',4,4'-tetrahydroxybenzophenone and the catalyst under continuous stirring. Stir well after addition, keep warm and stir for 6-8 hours, evaporate to remove low-boiling substances and solvent, separate the product, and vacuum dry it to obtain the cross-linking agent.
2. The colored LED-UV glass coating according to claim 1, characterized in that: The preparation method of the rigid hydrophilic monomer is as follows: 3-isopropyl-dimethylbenzyl isocyanate, sodium salt of N-hydroxysuccinimide sulfonic acid and toluene are added in sequence to a reaction bottle filled with nitrogen, stirring is started, and after a homogeneous solution is formed, the heating program is started and the temperature is raised to 70-80°C. The tin catalyst is then added to the bottle. After complete addition, the solution is kept warm for 2-4 hours under continuous stirring, and the solvent and low-boiling substances are evaporated. After purification, the product can obtain a rigid hydrophilic monomer.
3. The colored LED-UV glass coating according to claim 2, characterized in that: The molar ratio of the 3-isopropyl-dimethylbenzyl isocyanate to the sodium salt of N-hydroxysuccinimide sulfonic acid is 1:1-1.
2.
4. The colored LED-UV glass coating according to claim 2, characterized in that: The tin catalyst is at least one of dibutyltin didodecylsulfide, stannous octoate, dibutyltin dilaurate or dibutyltin diacetate.
5. The colored LED-UV glass coating according to claim 1, characterized in that: The average molecular weight of the epoxy-terminated allyl polyether is 450-1000.
6. The colored LED-UV glass coating according to claim 1, characterized in that: The catalyst is a boron trifluoride ether complex, and the amount of the catalyst added is 1-3% of the total mass of the epoxy-terminated allyl polyether and 2,2',4,4'-tetrahydroxybenzophenone.
7. The colored LED-UV glass coating according to claim 1, characterized in that: The initiator is benzoyl peroxide or dicumyl peroxide; the LED photoinitiator is at least one of photoinitiator 819, photoinitiator 907 or photoinitiator 369; the defoamer is BYK-1790 non-silicone defoamer; the leveling agent is an acrylate leveling agent; and the pigment is at least one of carbon black, iron red and Prussian blue.
8. The method for preparing a colored LED-UV glass coating according to claim 1, wherein: The following steps are involved: Step 1: Preparation of acrylate prepolymer Add half part by weight of methyl methacrylate, isobutyl acrylate, butyl acrylate, hydroxyethyl methacrylate and rigid hydrophilic monomer to purified water, stir and mix evenly, heat to 60-70°C, keep stirring for 2-4 hours, add the remaining amount of methyl methacrylate, isobutyl acrylate, butyl acrylate and hydroxyethyl methacrylate, and continue to add crosslinking agent and initiator, keep warm for 4-6 hours to form acrylate prepolymer; Step 2: Prepare glass coating Add leveling agent and pigment to acrylate prepolymer, stir and mix at a stirring rate of 800-1000 r / min for 20-30 minutes, add LED photoinitiator and defoamer, adjust the stirring rate to 300-500 r / min, and continue stirring for 5-10 minutes to prepare glass coating.
Citation Information
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