A silver mirror water-based mirror back paint and a preparation method thereof
By mixing modified waterborne acrylic resin and waterborne amino resin, a waterborne mirror back coating for silver mirrors was prepared, which solved the pollution and corrosion problems of traditional mirror back coatings, achieved a coating with high adhesion and durability, and extended the service life of the mirror.
Patent Information
- Application Number
- CN202410288891.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-03-14
- Publication Date
- 2025-11-07
- Estimated Expiration
- 2044-03-14
AI Technical Summary
Traditional mirror back paint is organic solvent-based, which poses a risk of pollution, has uneven coating, poor adhesion, and is prone to corrosion, affecting the quality and appearance of the mirror.
The preparation method of silver mirror water-based mirror back paint involves mixing modified water-based acrylic resin and water-based amino resin, adding components such as titanium dioxide, silicon dioxide, and zinc oxide, and combining them with wetting agents, defoamers, film-forming aids, etc., to form a corrosion-resistant coating.
It improves the adhesion and durability of the coating, prevents coating peeling and corrosion, extends the service life of the mirror, and has excellent corrosion resistance and stability.
Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to the technical field of water-based mirror back paint, in particular to a silver mirror water-based mirror back paint and a preparation method thereof. BACKGROUND
[0002] The silver mirror water-based mirror back paint is a coating used on the back of a mirror, which has the functions of moisture resistance, rust resistance, and oxidation resistance. During the production of a mirror, the back of the mirror needs to be coated to protect the surface of the mirror and the silver plating layer, while increasing the aesthetic and durability of the mirror. However, traditional mirror back paint is usually an organic solvent-based coating, containing volatile organic components, which can easily pollute the environment. At the same time, during the coating process, there may be problems such as uneven coating and poor adhesion, which can easily be corroded in a humid environment, causing spots or oxidation on the surface of the mirror, affecting the quality and appearance of the mirror.
[0003] Therefore, we propose a silver mirror water-based mirror back paint and a preparation method thereof. SUMMARY
[0004] The purpose of the present application is to provide a silver mirror water-based mirror back paint and a preparation method thereof to solve the problems raised in the background.
[0005] In order to solve the above technical problems, the present application provides the following technical scheme:
[0006] A preparation method of a silver mirror water-based mirror back paint, comprising the following steps:
[0007] Step S1: uniformly mix styrene, acrylic acid, butyl acrylate, N-hydroxymethyl acrylamide, methyl methacrylate, 2-acrylamido-2-methylpropanesulfonic acid, benzoyl peroxide, and propylene glycol methyl ether to obtain a mixed solution;
[0008] Step S2: heat the double bond-containing compound to 100-110°C, uniformly mix n-dodecanethiol and propylene glycol methyl ether, drop 1 / 5 mass fraction of the mixed solution, drop for 30-40 min, continue to drop the remaining mixed solution, drop for 2-3 h, add benzoyl peroxide solution, keep the reaction for 2-3 h, cool to 50-70°C, add triethylamine for neutralization for 50-60 min, add deionized water for emulsification to obtain a modified water-based acrylic resin;
[0009] Step S3: uniformly mix the modified water-based acrylic resin and the water-based amino resin, uniformly mix titanium dioxide, silicon dioxide, and deionized water, and then uniformly mix wetting agent, defoaming agent, film-forming aid, zinc oxide, methyl benzotriazole, and thickening agent to obtain the silver mirror water-based mirror back paint.
[0010] Further, the mixed solution in step S1 includes the following components by weight: styrene 12-14 parts, acrylic acid 2-4 parts, butyl acrylate 4-6 parts, N-methylol acrylamide 2-4 parts, methyl methacrylate 6-8 parts, 2-acrylamido-2-methylpropanesulfonic acid 3-5 parts, benzoyl peroxide 1-2 parts, and propylene glycol methyl ether 10-15 parts.
[0011] Further, the mass of the double-bond-containing compound in step S2 is 2.5-3.0 times the mass of the styrene.
[0012] Further, the mass of n-dodecanethiol in step S2 is 3-5% of the mass of the double-bond-containing compound.
[0013] Further, the mass of propylene glycol methyl ether in step S2 is 0.3-0.5 times the mass of the double-bond-containing compound.
[0014] Further, the benzoyl peroxide solution in step S2 is prepared by mixing benzoyl peroxide and deionized water in a mass ratio of 1:(8-10), and the mass of the benzoyl peroxide is 2-4% of the mass of the double-bond-containing compound.
[0015] Further, the mass of the deionized water in step S2 is 3-4 times the mass of the double-bond-containing compound.
[0016] Further, the preparation method of the double-bond-containing compound in step S2 is as follows:
[0017] Step (1): uniformly mix bisphenol A (2,3-dihydroxypropyl) glycidyl ether, palmitoleic acid, and tetrabutylammonium bromide, heat to 125-135°C, react for 5-7 h, cool to room temperature, wash and dry to obtain a modified polyol;
[0018] Step (2): uniformly mix linolenic acid, the modified polyol, and phthalic anhydride under nitrogen protection, add dimethylbenzene and hypophosphorous acid, heat to 145-155°C, heat for 1-2 h, continue to heat at a heating rate of (0.3-0.5) °C / min to 205-225°C, react for 4-6 h, heat to 235-245°C, uniformly mix 4-methoxyphenol and N-(methoxymethyl)-2-propenamide, react for 3-5 h, cool to room temperature to obtain the double-bond-containing compound.
[0019] In the above technical scheme, under the catalysis of tetrabutylammonium bromide, the bisphenol A (2, 3-dihydroxypropyl) glycidyl ether is subjected to an epoxy ring-opening reaction with palmitoleic acid to generate a hydroxyl group, thereby obtaining a modified polyol; linolenic acid is selected as a fatty acid, phthalic anhydride is selected as a polyacid, and the modified polyol is subjected to a reaction, and then N- (methoxymethyl) -2-propenamide is further reacted with the hydroxyl group on the alkyd resin to introduce a double bond, thereby obtaining a double bond-containing compound.
[0020] Further, in the step (1), the mass ratio of the bisphenol A (2, 3-dihydroxypropyl) glycidyl ether, the palmitoleic acid and the tetrabutylammonium bromide is 1: (0.7-0.9) : (0.01-0.03).
[0021] Further, in the step (2), the mass ratio of the linolenic acid, the modified polyol and the phthalic anhydride is 1: (0.8-1.0) : (0.4-0.5).
[0022] Further, in the step (2), the mass of the xylene is 8-10% of the total mass of the linolenic acid, the modified polyol and the phthalic anhydride.
[0023] Further, in the step (2), the mass of the hypophosphorous acid is 0.1-0.3% of the mass of the linolenic acid.
[0024] Further, in the step (2), the mass of the 4-methoxyphenol is 6-10% of the mass of the N- (methoxymethyl) -2-propenamide.
[0025] Further, in the step (2), the mass of the N- (methoxymethyl) -2-propenamide is 20-30% of the mass of the modified polyol.
[0026] Further, the silver mirror water-based mirror back paint comprises the following components by weight: 40-60 parts of modified water-based acrylic resin, 10-20 parts of water-based amino resin, 3-15 parts of deionized water, 5-10 parts of titanium white, 10-20 parts of silicon dioxide, 5-10 parts of zinc oxide, 10-15 parts of methyl benzotriazole, 0.2-0.4 parts of wetting agent, 0.1-0.3 parts of defoaming agent, 2-4 parts of film-forming aid, and 0.1-0.2 parts of thickening agent.
[0027] Further, the silicon dioxide is subjected to surface modification, and the specific modification process is as follows:
[0028] The silicon dioxide, 3-glycidylpropyltrimethoxysilane and ethanol are uniformly mixed, heated to 50-60℃, and reacted for 5-6h, and then washed and dried to obtain modified silicon dioxide.
[0029] In the above technical solution, the surface of the silica is modified by 3-glycidylpropyltrimethoxysilane, which not only improves the dispersion uniformity of the silica, but also improves the wear resistance of the paint film.
[0030] Further, the mass ratio of the silica, 3-glycidylpropyltrimethoxysilane and ethanol is 1:
[0031] (0.2-0.4) : (6-8).
[0032] Further, the film-forming aid is composed of 1-2 parts by mass of dipropylene glycol butyl ether and 1-2 parts by mass of ethylene glycol monobutyl ether.
[0033] Compared with the prior art, the present application has the following advantages:
[0034] 1. A silver mirror water-based mirror back paint and a preparation method thereof, under the catalysis of tetrabutylammonium bromide, a modified polyol is obtained by using palmitoleic acid to perform an epoxy ring-opening reaction on bisphenol A (2,3-dihydroxypropyl) glycidyl ether to generate a hydroxyl group; a fatty acid selected from linolenic acid is reacted with the modified polyol, and phthalic anhydride is used as a polyacid; then N-(methoxymethyl)-2-propenamide is further reacted with the hydroxyl group on the alkyd resin to introduce a double bond and an NH group, thereby obtaining a double bond-containing compound; under the action of an initiator, the double bond-containing compound is polymerized with acrylic acid, butyl acrylate, N-hydroxymethyl acrylamide, methyl methacrylate and 2-acrylamido-2-methylpropane sulfonic acid to introduce an NH group and a sulfonate group, thereby obtaining a modified water-based acrylic resin with excellent corrosion resistance.
[0035] 2. A silver mirror water-based mirror back paint and a preparation method thereof, the silver mirror water-based mirror back paint is obtained by mixing the modified water-based acrylic resin and a water-based amino resin, adding titanium dioxide and silicon dioxide as fillers, zinc oxide and methylbenzotriazole as corrosion inhibitors, and combining the effects of a wetting agent, a defoaming agent, a film-forming aid, a thickening agent and deionized water, which not only can provide excellent coating performance, increase the adhesion and durability of the mirror back paint, effectively prevent the coating from falling off and corrosion, thereby prolonging the service life of the mirror, but also has excellent corrosion resistance, which can ensure that the coating remains stable and durable for a long time. DETAILED DESCRIPTION
[0036] The technical solutions in the embodiments of the present application will be described below in a clear and complete manner. Obviously, the described embodiments are only some of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.
[0037] The waterborne amino resin in this embodiment: item number AA-9077, from Suzhou Qingtian New Material Co., Ltd.; titanium dioxide: DHA-100 sharp titanium type, particle size 20-50 nm, from Shanghai Leifu International Trade Co., Ltd.; silicon dioxide: item number PST-H20, particle size 20 nm, from Nanjing Baokete New Material Co., Ltd.; zinc oxide: model KND-NX10, particle size 10-30 nm, from Changzhou Kenada New Material Technology Co., Ltd.; methyl benzotriazole: item number EF234243, from Wuhan Lanya Bai Pharmaceutical Chemical Co., Ltd.; wetting agent: item number BYK-P104S, from Huizhou Aike New Material Co., Ltd.; defoaming agent: model BYK-028, from Dongguan Haoyouduo New Material Co., Ltd.; thickening agent: model ASE-60, from Wuxi Handerson Chemical Co., Ltd.
[0038] In the following examples and comparative examples, 1 part is equal to 10 g.
[0039] Example 1: A preparation method of a silver mirror waterborne mirror back paint, comprising the following processes:
[0040] Step S1: uniformly mix 12 parts of styrene, 2 parts of acrylic acid, 4 parts of butyl acrylate, 2 parts of N-hydroxymethyl acrylamide, 6 parts of methyl methacrylate, 3 parts of 2-acrylamido-2-methylpropane sulfonic acid, 1 part of benzoyl peroxide, and 10 parts of propylene glycol methyl ether to obtain a mixed solution;
[0041] Step S2: uniformly mix 30 parts of a double bond-containing compound at 100°C, add 0.9 parts of n-dodecanethiol and 9 parts of propylene glycol methyl ether, drop 1 / 5 mass fraction of the mixed solution, drop for 30 min, continue to drop the remaining mixed solution, drop for 2 h, add a benzoyl peroxide solution (mixed by 0.6 parts of benzoyl peroxide and 4.8 parts of water), keep warm for 2 h, cool to 50°C, add triethylamine for neutralization for 50 min, add 90 parts of deionized water for emulsification, to obtain a modified waterborne acrylic resin;
[0042] Step S3: uniformly mix 40 parts of the modified waterborne acrylic resin and 10 parts of the waterborne amino resin, add 5 parts of titanium dioxide, 10 parts of silicon dioxide, 3 parts of deionized water, and uniformly mix, then add 0.2 parts of a wetting agent, 0.1 parts of a defoaming agent, 1 parts of dipropylene glycol butyl ether, 1 parts of ethylene glycol monobutyl ether, 5 parts of zinc oxide, 10 parts of methyl benzotriazole, and 0.1 parts of a thickening agent, and uniformly mix, to obtain a silver mirror waterborne mirror back paint;
[0043] The preparation method of the double bond-containing compound is as follows:
[0044] Step (1): 30 parts of bisphenol A (2,3-dihydroxypropyl) glycidyl ether, 21 parts of palmitoleic acid and 0.3 parts of tetrabutylammonium bromide were uniformly mixed, heated to 125℃, reacted for 5h, cooled to room temperature, washed and dried to obtain a modified polyol;
[0045] Step (2): 37.5 parts of linolenic acid, 30 parts of modified polyol, 15 parts of phthalic anhydride were uniformly mixed, 6.6 parts of xylene and 0.04 parts of hypophosphorous acid were added, heated to 145℃, kept for 1h, continued to heat to 205℃ at a heating rate of 0.1℃ / min, reacted for 4h, heated to 235℃, added 0.36 parts of 4-methoxyphenol and 6 parts of N-(methoxymethyl)-2-propenamide and mixed uniformly, reacted for 3h, cooled to room temperature to obtain a double bond-containing compound;
[0046] The silica was surface modified, and the specific modification process was as follows:
[0047] 10 parts of silica and 2 parts of 3-glycidylpropyltrimethoxysilane, 60 parts of ethanol were uniformly mixed, heated to 50℃, reacted for 5h, washed and dried to obtain modified silica.
[0048] Example 2: A preparation method of a silver mirror water-based mirror back paint, comprising the following processes:
[0049] Step S1: 13 parts of styrene, 3 parts of acrylic acid, 5 parts of butyl acrylate, 3 parts of N-hydroxymethyl acrylamide, 7 parts of methyl methacrylate, 4 parts of 2-acrylamido-2-methylpropane sulfonic acid, 1.5 parts of benzoyl peroxide, 12 parts of propylene glycol methyl ether were uniformly mixed to obtain a mixed solution;
[0050] Step S2: 35 parts of a double bond-containing compound was heated to 105℃, 1.4 parts of n-dodecanethiol, 14 parts of propylene glycol methyl ether were uniformly mixed, 1 / 5 mass fraction of the mixed solution was added dropwise, and the dropwise addition was completed in 35min, the remaining mixed solution was continuously added dropwise, and the dropwise addition was completed in 2.5h, benzoyl peroxide solution (prepared by mixing 1 part of benzoyl peroxide and 9 parts of water) was added, and the reaction was kept for 2.5h, the temperature was lowered to 60℃, triethylamine was added for neutralization for 55min, deionized water was added for emulsification to obtain a modified water-based acrylic resin;
[0051] Step S3: 50 parts of modified water-based acrylic resin and 15 parts of water-based amino resin were uniformly mixed, 8 parts of titanium white, 15 parts of silica, 10 parts of deionized water were uniformly mixed, and then 0.3 parts of wetting agent, 0.2 parts of defoaming agent, 1.5 parts of dipropylene glycol butyl ether, 1.5 parts of ethylene glycol monobutyl ether, 8 parts of zinc oxide, 12 parts of methyl benzotriazole, and 0.15 parts of thickening agent were uniformly mixed to obtain a silver mirror water-based mirror back paint.
[0052] The preparation method of the double bond-containing compound is as follows:
[0053] Step (1): 35 parts of bisphenol A (2,3-dihydroxypropyl) glycidyl ether, 28 parts of palmitoleic acid, and 0.7 parts of tetrabutylammonium bromide are uniformly mixed, heated to 130°C, reacted for 6h, cooled to room temperature, washed and dried to obtain a modified polyol;
[0054] Step (2): 35 parts of linoleic acid, 32 parts of modified polyol, and 16 parts of phthalic anhydride are uniformly mixed under nitrogen protection, 7.5 parts of xylene and 0.07 parts of hypophosphorous acid are added, heated to 150°C, and kept for 1.5h, then heated to 210°C at a heating rate of 0.4°C / min, reacted for 5h, heated to 240°C, added 0.7 parts of 4-methoxyphenol and 8 parts of N-(methoxymethyl)-2-propenamide, mixed uniformly, reacted for 4h, and cooled to room temperature to obtain a double bond-containing compound.
[0055] The surface of the silicon dioxide is modified, and the specific modification process is as follows:
[0056] 15 parts of silicon dioxide and 4.5 parts of 3-glycidylpropyltrimethoxysilane, 105 parts of ethanol are uniformly mixed, heated to 55°C, reacted for 5.5h, washed and dried to obtain modified silicon dioxide.
[0057] Example 3: A preparation method of a silver mirror water-based mirror back paint, comprising the following processes:
[0058] Step S1: 14 parts of styrene, 4 parts of acrylic acid, 6 parts of butyl acrylate, 4 parts of N-hydroxymethyl acrylamide, 8 parts of methyl methacrylate, 5 parts of 2-acrylamido-2-methylpropane sulfonic acid, 2 parts of benzoyl peroxide, and 15 parts of propylene glycol methyl ether are uniformly mixed to obtain a mixed solution;
[0059] Step S2: 42 parts of the double bond-containing compound is heated to 110°C, 2.1 parts of n-dodecanethiol, 21 parts of propylene glycol methyl ether are uniformly mixed, 1 / 5 mass fraction of the mixed solution is added dropwise, and the dropwise addition is completed in 40min, the remaining mixed solution is continuously added dropwise, and the dropwise addition is completed in 3h, the benzoyl peroxide solution (prepared by mixing 1.68 parts of benzoyl peroxide and 16.8 parts of water) is added, and the reaction is kept for 3h, the temperature is lowered to 70°C, triethylamine is added and neutralized for 60min, deionized water is added for emulsification to obtain a modified water-based acrylic resin;
[0060] Step S3: 60 parts of modified water-based acrylic resin and 20 parts of water-based amino resin are mixed uniformly, 10 parts of titanium white powder, 20 parts of silicon dioxide, 15 parts of deionized water are mixed uniformly, and then 0.4 parts of wetting agent, 0.3 parts of defoaming agent, 2 parts of dipropylene glycol butyl ether, 2 parts of ethylene glycol monobutyl ether, 10 parts of zinc oxide, 15 parts of methyl benzotriazole, and 0.2 parts of thickening agent are mixed uniformly to obtain a silver mirror water-based mirror back paint;
[0061] The preparation method of the double bond-containing compound is as follows:
[0062] Step (1): 42 parts of bisphenol A (2,3-dihydroxypropyl) glycidyl ether, 37.8 parts of palmitoleic acid, and 1.26 parts of tetrabutylammonium bromide are mixed uniformly, heated to 135℃, reacted for 7h, cooled to room temperature, washed and dried to obtain a modified polyol;
[0063] Step (2): Under the protection of nitrogen, 42 parts of linolenic acid, 42 parts of modified polyol, and 21 parts of phthalic anhydride are mixed uniformly, 10.5 parts of xylene and 0.126 parts of hypophosphorous acid are added, heated to 155℃, and kept for 2h, then heated to 225℃ at a heating rate of 0.5℃ / min, reacted for 6h, heated to 245℃, and then 1.26 parts of 4-methoxyphenol and 12.6 parts of N-(methoxymethyl)-2-propenamide are mixed uniformly, reacted for 3-5h, and cooled to room temperature to obtain a double bond-containing compound.
[0064] The surface of the silicon dioxide is modified, and the specific modification process is as follows:
[0065] The modified silicon dioxide is obtained by mixing 20 parts of silicon dioxide, 8 parts of 3-glycidylpropyltrimethoxysilane, and 160 parts of ethanol uniformly, heating to 60℃, and reacting for 6h, and then washing and drying.
[0066] Comparative Example 1: The silver mirror water-based mirror back paint comprises the following components by weight: water-based acrylic resin 40 parts, water-based amino resin 10 parts, deionized water 3 parts, titanium white powder 5 parts, silicon dioxide 10 parts, zinc oxide 5 parts, methyl benzotriazole 10 parts, wetting agent 0.2 parts, defoaming agent 0.1 parts, and film forming agent 2 parts. Compared with Example 1, Comparative Example 1 adds the same mass of water-based acrylic resin (product number AA-8672S, from Suzhou Qingtian New Material Co., Ltd.), and the other steps and processes are the same as those of Example 1.
[0067] Comparative Example 2: The silver mirror water-based mirror back paint comprises the following components by weight: water-based acrylic resin 40 parts, deionized water 3 parts, titanium white powder 5 parts, silicon dioxide 10 parts, zinc oxide 5 parts, methyl benzotriazole 10 parts, wetting agent 0.2 parts, defoaming agent 0.1 parts, and film forming agent 2 parts. Comparative Example 2 does not add water-based amino resin, and the other steps and processes are the same as those of Example 1.
[0068] Preparation method of a silver mirror water-based mirror back paint, comprising the following processes:
[0069] Compared with Example 2, the preparation method of the silver mirror water-based mirror back paint of Comparative Example 3 does not include the preparation method of the double-bond-containing compound, and the double-bond-containing compound in step S2 is replaced by the same mass of hydroxyethyl acrylate, and the other steps are the same as those of Example 2.
[0070] Preparation method of a silver mirror water-based mirror back paint, comprising the following processes:
[0071] The preparation method of the double-bond-containing compound is as follows:
[0072] Step (1): 35 parts of bisphenol A (2,3-dihydroxypropyl) glycidyl ether, 28 parts of palmitoleic acid, and 0.7 parts of tetrabutylammonium bromide are uniformly mixed, heated to 130°C, reacted for 6h, cooled to room temperature, and after washing and drying, a modified polyol is obtained;
[0073] Step (2): 35 parts of linolenic acid, 32 parts of modified polyol, 16 parts of phthalic anhydride, 7.5 parts of xylene, and 0.07 parts of hypophosphorous acid are uniformly mixed under nitrogen protection, heated to 150°C, and kept for 1.5h, and then heated to 210°C at a heating rate of 0.4°C / min, reacted for 5h, heated to 240°C, and then 0.7 parts of 4-methoxyphenol and 6.4 parts of N-(methoxymethyl)-2-propenamide are uniformly mixed and reacted for 4h, and then cooled to room temperature to obtain a double-bond-containing compound;
[0074] Compared with Example 2, the mass of N-(methoxymethyl)-2-propenamide in step (2) of Comparative Example 4 is 10% of the mass of the modified polyol; and the other steps are the same as those of Example 2.
[0075] Experiment: The silver mirror water-based mirror back paints obtained in Examples 1-3 and Comparative Examples 1-4 are coated on the mirror back, and after baking and curing at 150°C for 10min, samples are prepared, and the performance of the samples is detected and the detection results are recorded:
[0076] The hardness is determined according to GB / T 6739-2022 “Pencil method for determining the hardness of paint film of color paint and varnish”, and the steps are as follows: the hardness is determined by using a QHQ-A portable pencil hardness tester, the same hardness pencil is used to test the sample surface for five times, and a pencil with a lower hardness is used until less than two scratches appear, and the hardness of the pencil is used as the hardness of the coating.
[0077] Adhesion was determined according to GB / T 9286-2021 "Color paint and varnish cross-cut test", and the experimental procedure was as follows: holding the cutting tool, making the blade perpendicular to the sample surface, using a 1mm spacing guide device, uniformly applying force to the cutting tool, and cutting 6 times on the coating at a uniform speed; then making 6 parallel cuts, intersecting the previous cuts at a 90 angle to form a grid pattern, visually inspecting the cutting area, and rating, 0 grade: the cutting edge is completely smooth, and there is no falling in the grid; 1 grade: there is a little coating falling at the intersection of the cuts, but the affected intersection cutting area is not more than 5%; 2 grade: there is coating falling at the intersection of the cuts and / or along the edge of the cuts, and the affected intersection cutting area is more than 5% but not more than 15%.
[0078] Corrosion resistance was determined according to GB / T1771-2007 "Varnish, color paint resistance to neutral salt spray test", and the experimental procedure was as follows: placing the sample in a salt spray chamber, the test solution was a 5% NaCl solution by mass fraction, observing the sample every 24h, whether there was bubbling, corrosion and other phenomena, and determining three coatings in parallel.
[0079] Test results
[0080] hardness adhesion corrosion pattern example 1 3H 0 level no apparent change in surface example 2 3H 0 level no apparent change in surface example 3 3H 0 level no apparent change in surface comparative example 1 H 2 level peeling phenomenon occurred comparative example 2 2H 2 level slight corrosion comparative example 3 H 2 level bubbling occurred comparative example 4 2H 1 level slight corrosion
[0081] According to the data in the above table, the following conclusions can be clearly obtained:
[0082] 1. Compared with examples 1-3, the product of comparative example 1 showed a decrease in hardness, adhesion and corrosion resistance, indicating that the modified water-based acrylic resin prepared by the present application has better performance compared with water-based acrylic resin.
[0083] 2. Compared with examples 1-3, the products obtained in comparative examples 2 and 3 showed a decrease in hardness, adhesion and corrosion resistance, which indicated that the addition of water-based amino resin in the present application increased the crosslinking density of the coating, thereby improving the hardness, adhesion and corrosion resistance of the coating; at the same time, compared with hydroxyethyl acrylate, the double bond containing compound prepared by the present application can better improve the comprehensive performance of the water-based acrylic resin.
[0084] 3. Compared with examples 1-3, the product of comparative example 4 showed a decrease in hardness, adhesion and corrosion resistance, which indicated that the performance of the double bond containing compound prepared by the present application was affected by the ratio of each reagent in the preparation process, and the water-based mirror back paint prepared by selecting the mass ratio within the range had excellent hardness and corrosion resistance, thereby prolonging the service life of the silver mirror.
[0085] It is to be noted that, in the present text, relationai terminology, such as first and second, and the like, is used merely to distinguish one entity or action from another entity or action, and is not necessarily intended to or should be construed to imply that such entity or action is in any way superior, lower, or more important in relation to the other entities or actions so distinguished. Furthermore, the terms "comprising", "containing", or any other open-ended variant thereof are intended to cover a non-exclusive inclusion, such that processes methods articles or apparatuses that comprise a list of elements are not limited to those elements but can include other elements not expressly listed or inherent to such processes methods articles or apparatuses.
[0086] Finally, it should be noted that the above-mentioned only indicates the preferred embodiments of the present application, and is not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications, equivalent replacements or improvements of the technical solutions described in the foregoing embodiments can be made. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims
1. A process for the preparation of a silver mirror aqueous mirror backing paint, characterized by: It comprises the following steps: Step S1: uniformly mix styrene, acrylic acid, butyl acrylate, N-hydroxymethyl acrylamide, methyl methacrylate, 2-acrylamido-2-methylpropanesulfonic acid, benzoyl peroxide, and propylene glycol methyl ether to obtain a mixed solution; Step S2: heat the double bond-containing compound to 100-110℃, uniformly mix n-dodecanethiol and propylene glycol methyl ether, drop 1 / 5 mass fraction of the mixed solution, drop for 30-40min, continue to drop the remaining mixed solution, drop for 2-3h, add benzoyl peroxide solution, incubate for 2-3h, cool to 50-70℃, add triethylamine for neutralization for 50-60min, add deionized water for emulsification to obtain a modified water-based acrylic resin; Step S3: uniformly mix the modified water-based acrylic resin and the water-based amino resin, add titanium dioxide, silicon dioxide, and deionized water, and then uniformly mix wetting agent, defoaming agent, film-forming aid, zinc oxide, methyl benzotriazole, and thickening agent to obtain a silver mirror water-based mirror back paint; The preparation method of the double bond-containing compound in step S2 is as follows: Step (1): uniformly mix bisphenol A (2,3-dihydroxypropyl) glycidyl ether, palmitoleic acid, and tetrabutylammonium bromide, heat to 125-135℃, react for 5-7h, cool to room temperature, and then wash and dry to obtain a modified polyol; Step (2): under nitrogen protection, uniformly mix linolenic acid, modified polyol, and phthalic anhydride, add xylene and hypophosphorous acid, heat to 145-155℃, incubate for 1-2h, continue to heat to 205-225℃ at a heating rate of 0.3-0.5℃ / min, react for 4-6h, heat to 235-245℃, uniformly mix 4-methoxyphenol and N-(methoxymethyl)-2-propenamide, and react for 3-5h to obtain the double bond-containing compound.
2. The method for preparing a silver mirror water-based mirror backing paint according to claim 1, characterized in that: The mixed solution in step S1 comprises the following components by weight: styrene 12-14 parts, acrylic acid 2-4 parts, butyl acrylate 4-6 parts, N-hydroxymethyl acrylamide 2-4 parts, methyl methacrylate 6-8 parts, 2-acrylamido-2-methylpropanesulfonic acid 3-5 parts, benzoyl peroxide 1-2 parts, and propylene glycol methyl ether 10-15 parts.
3. The method for preparing a silver mirror water-based mirror backing paint according to claim 1, characterized in that: The mass ratio of bisphenol A (2,3-dihydroxypropyl) glycidyl ether, palmitoleic acid, and tetrabutylammonium bromide in step (1) is 1:(0.7-0.9):(0.01-0.03).
4. The method for preparing a silver mirror water-based mirror backing paint according to claim 1, characterized in that: The mass ratio of linolenic acid, modified polyol, and phthalic anhydride in step (2) is 1:(0.8-1.0):(0.4-0.5).
5. The method for preparing a silver mirror water-based mirror backing paint according to claim 1, characterized in that: The silver mirror water-based mirror back paint comprises the following components by weight: modified water-based acrylic resin 40-60 parts, water-based amino resin 10-20 parts, deionized water 3-15 parts, titanium dioxide 5-10 parts, silicon dioxide 10-20 parts, zinc oxide 5-10 parts, methyl benzotriazole 10-15 parts, wetting agent 0.2-0.4 parts, defoaming agent 0.1-0.3 parts, film-forming aid 2-4 parts, and thickening agent 0.1-0.2 parts.
6. The method for preparing a silver mirror water-based mirror backing paint according to claim 5, characterized in that: The silica is surface modified, and the specific modification process is as follows: The silica, 3-glycidylpropyltrimethoxysilane and ethanol are uniformly mixed, heated to 50-60 DEG C, and reacted for 5-6 hours, and then washed and dried to obtain the modified silica.
7. The method for preparing a silver mirror water-based mirror backing paint according to claim 6, characterized in that: The mass ratio of the silica, 3-glycidylpropyltrimethoxysilane and ethanol is 1:(0.2-0.4):(6-8).
8. The method for preparing a silver mirror water-based mirror backing paint according to claim 5, characterized in that: The film forming aid is composed of 1-2 parts by mass of dipropylene glycol butyl ether and 1-2 parts by mass of ethylene glycol monobutyl ether.
9. A silver mirror aqueous mirror back paint prepared by the preparation method according to any one of claims 1-8.
Citation Information
Patent Citations
Aqueous alkide resin-acrylic acid resin hybrid coating and preparation method thereof
CN103725145A