A water-based printing paint, a preparation method and application thereof

Abstract

The application provides a water-based printing paint, a preparation method and application thereof, and belongs to the technical field of paints.The water-based printing paint comprises the following raw materials: 55-65 parts by weight of a water-based resin emulsion, 1-2 parts by weight of an adhesion promoter, 0.7-1.2 parts by weight of a water-based dispersing agent, 0.3-0.6 parts by weight of a water-based defoaming agent, 1-3 parts by weight of a film-forming aid and 30-40 parts by weight of water; wherein the adhesion promoter is prepared from hydroxypropyl acrylate, isomeric tridecanol polyoxyethylene ether, gamma-aminopropyl triethoxysilane and alkenyl grafted phytic acid.The water-based printing paint prepared by the application meets the green environmental protection requirement, has low VOC content, good printing effect, excellent adhesion and wear resistance.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of coatings, and particularly relates to a water-based printing coating, a preparation method and application thereof. BACKGROUND

[0002] Printing coatings are an integral part of modern printing technology, playing a key role in enhancing the quality and functionality of printed materials. From books and magazines to packaging materials, from advertising posters to art reproductions, almost any item that requires printing can be enhanced in its physical properties and visual appeal through the use of different printing coatings. Printing coatings can be divided into various types, including water-based coatings, oil-based coatings, UV ultraviolet curing coatings, etc., each with its unique advantages and application scope. For example, water-based coatings are particularly suitable for children's books and food packaging due to their environmentally friendly and non-toxic characteristics; while UV coatings are known for their fast drying, high strength gloss, and excellent wear resistance, making them ideal for high-end packaging and promotional materials. To achieve the best coating effect, printing coatings can be applied to the substrate through various methods such as coating, spraying, roller transfer, screen printing, etc., ensuring uniform and consistent coating and tight bonding with the substrate, thereby improving the wear resistance, durability, and stain resistance of the printed material.

[0003] With the increasing awareness of environmental protection, the printing industry has increasingly high requirements for green printing technology. Environmentally friendly coatings not only reduce the emission of volatile organic compounds (VOC) and energy consumption, but also ensure that product quality is not affected. Currently, water-based printing coatings have relatively poor adhesion performance, especially on non-polar or smooth substrates such as plastics and metals, etc., and the coating film is prone to peeling or delamination, which not only affects the aesthetic appearance of the product, but also reduces its protective function. The toughness of the coating film formed by water-based coatings is not high, and it is prone to cracking under mechanical stress such as bending and folding, resulting in poor durability. In addition, water-based coatings have poor wear resistance and are difficult to resist daily use friction and scratches, which is a significant disadvantage for products that require frequent contact, such as packaging materials and promotional materials.

[0004] To overcome the above-mentioned shortcomings of water-based printing coatings, various methods have been used in the prior art to improve these properties. For example, by optimizing the formula, adding functional additives such as cross-linking agents, plasticizers and surfactants, the adhesion and toughness of water-based coatings can be improved to a certain extent; cross-linking agents can form a three-dimensional network structure during the drying process of the coating film, enhancing the mechanical strength and chemical resistance of the coating film, plasticizers help to improve the flexibility and impact resistance of the coating film, and surfactants can reduce the surface tension of water, promoting better wetting of the substrate by the coating, thereby improving adhesion. Secondly, the substrate can also be pretreated by corona treatment or flame treatment to increase the energy of the substrate surface and improve the affinity between the coating and the substrate. For materials such as plastics that are difficult to adhere, primer or coating treatment can provide a better adhesion interface for water-based coatings. However, despite the above measures, there are still some shortcomings, such as the addition of too many additives which can cause the hardness of the coating film to decrease, affecting its wear resistance and gloss, and the pretreatment of the substrate increases the production steps and costs, affecting the efficiency of large-scale production. Therefore, there is an urgent need for a water-based printing coating with low VOC content and excellent adhesion and wear resistance. SUMMARY

[0005] The purpose of the present application is to provide a water-based printing coating that uses a specific water-based resin emulsion and an adhesion promoter to make the printing coating not only environmentally friendly and low in VOC content, but also has excellent adhesion and wear resistance. The present application also provides a method for preparing the above-mentioned water-based printing coating and its application in digital inkjet printing.

[0006] To achieve the above-mentioned purpose, the present application provides the following technical solutions:

[0007] The present application provides a water-based printing coating, comprising the following raw materials by weight:

[0008] 55-65 parts by weight of water-based resin emulsion, 1-2 parts by weight of adhesion promoter, 0.7-1.2 parts by weight of water-based dispersant, 0.3-0.6 parts by weight of water-based defoamer, 1-3 parts by weight of film-forming aid, 30-40 parts by weight of water.

[0009] Preferably, the preparation method of the water-based resin emulsion comprises the following steps:

[0010] Mix 5-8 parts by weight of polyvinyl alcohol, 2-5 parts by weight of epichlorohydrin and 80-100 parts by weight of hydrochloric acid, heat and stir, centrifuge, dry to obtain an intermediate; mix 3-5 parts by weight of the intermediate, 0.03-0.06 parts by weight of tetrabutylammonium bromide and 40-60 parts by weight of ammonia water, then add 15-25 parts by weight of ethylenediamine, heat and stir, centrifuge, dry to obtain aminated polyvinyl alcohol;

[0011] Mixing 8-12 parts by weight of ethyl orthosilicate, 20-30 parts by weight of aluminum nitrate and 100-150 parts by weight of anhydrous ethanol to obtain a mixed solution, adding the mixed solution into 150-200 parts by weight of ammonia water under stirring to react, filtering, drying, and calcining to obtain a silica / alumina composite; mixing 5-7 parts by weight of the silica / alumina composite with 40-60 parts by weight of water under stirring, then adding 1-1.5 parts by weight of 3-acrylamidopropyl tris(trimethylsiloxy)silane, continuing to stir under heating, cooling, filtering, and drying to obtain a surface-modified silica / alumina composite;

[0012] Mixing 0.2-0.5 parts by weight of sodium dodecyl sulfate, 0.08-0.12 parts by weight of polyvinylpyrrolidone with 10-20 parts by weight of water, then adding 2-5 parts by weight of the surface-modified silica / alumina composite and 1-4 parts by weight of aminated polyvinyl alcohol under ultrasonic dispersion, and then adding 6-8 parts by weight of ethyl methacrylate, 2-4 parts by weight of butyl acrylate and 0.05-0.15 parts by weight of ammonium persulfate to react under heating in a nitrogen atmosphere to obtain an intermediate material; mixing 2-4 parts by weight of acrylic acid, 6-8 parts by weight of ethyl methacrylate, 1-4 parts by weight of butyl acrylate, 1-2 parts by weight of hydroxypropyl acrylate, 0.3-0.8 parts by weight of methacrylamide and 0.1-0.3 parts by weight of ammonium persulfate, stirring under heating, then adding 10-30 parts by weight of the intermediate material to continue stirring, and cooling to obtain an aqueous resin emulsion.

[0013] The above aqueous resin emulsion prepared by the present application not only can maintain good adhesion of the aqueous printing paint, but also can further improve the wear resistance of the paint, thereby prolonging the service life. In the preparation process, acrylic acid, ethyl methacrylate, butyl acrylate, hydroxypropyl acrylate and methacrylamide components are used as the matrix, and the surface-modified silica / alumina composite and aminated polyvinyl alcohol are used as the functional filler, so that the wear resistance of the paint is significantly improved while maintaining good adhesion.

[0014] Firstly, the silica / alumina composite is obtained by sol-gel method using the precursor tetraethyl orthosilicate and aluminum nitrate. Compared with silica, the introduction of alumina into the composite can assist in enhancing the wear resistance of the filler. The surface of the silica / alumina composite is modified with 3-acrylamidopropyl tri(trimethylsiloxy) silane, which not only improves the surface activity, but also enhances the binding force and adhesion between the filler and the emulsion matrix component, effectively preventing the filler from falling off during use, thereby further improving the wear resistance of the coating. Secondly, the surface-modified silica / alumina composite is used as the core, and ethyl methacrylate and butyl acrylate are used as the shell monomer. The core-shell emulsion is obtained by emulsion polymerization, and the introduction of hydroxypropyl acrylate and methacrylamide monomers in the system promotes the formation of a cross-linked network, which plays a role in fixing and bonding the silica / alumina composite. This cross-linked network not only enhances the binding force between the composite and the matrix component, but also provides a physical protective layer, further improving the wear resistance of the coating.

[0015] In addition, amino polyvinyl alcohol is added as a reinforcing filler. After aminoization, the polyvinyl alcohol can be connected to the acrylate backbone through polymerization of the active functional groups on the acrylate monomers and the amino groups. This not only improves the flexibility and wear resistance of the coating, but also enhances the binding performance between the components through hydrogen bonding and other interaction forces. Amino polyvinyl alcohol has good film-forming properties and hydrophilicity, making the coating have better wear resistance while maintaining excellent adhesion performance, enhancing the adhesion between the coating and the substrate, and reducing the risk of coating peeling.

[0016] Further, the preparation method of the water-based resin emulsion comprises the following steps:

[0017] Mix 5-8 parts by weight of polyvinyl alcohol, 2-5 parts by weight of epichlorohydrin and 80-100 parts by weight of 0.2-0.5wt% hydrochloric acid, stir at 65-70℃ and 100-200rpm for 40-60min, centrifuge, dry to obtain an intermediate; mix 3-5 parts by weight of the intermediate, 0.03-0.06 parts by weight of tetrabutylammonium bromide and 40-60 parts by weight of 0.3-0.6wt% ammonia water, then add 15-25 parts by weight of ethylenediamine, stir at 65-70℃ and 100-200rpm for 2-4h, centrifuge, dry to obtain amino polyvinyl alcohol;

[0018] Mixing 8-12 parts by weight of ethyl orthosilicate, 20-30 parts by weight of aluminum nitrate and 100-150 parts by weight of anhydrous ethanol to obtain a mixed solution, adding the mixed solution into 150-200 parts by weight of 15-18 wt% ammonia water under the conditions of 30-40°C and 500-700 rpm stirring, and reacting for 6-8 hours, filtering, drying, and then calcining at 450-550°C for 2-4 hours to obtain a silica / alumina composite; mixing 5-7 parts by weight of the silica / alumina composite and 40-60 parts by weight of water under the conditions of room temperature and 500-700 rpm stirring for 0.3-0.6 hours, then adding 1-1.5 parts by weight of 3-acrylamidopropyl tris(trimethylsiloxy) silane, and continuing to stir at 85-90°C for 10-15 hours, and then cooling to room temperature, filtering, and drying to obtain a surface-modified silica / alumina composite;

[0019] Mixing 0.2-0.5 parts by weight of sodium dodecyl sulfate, 0.08-0.12 parts by weight of polyvinylpyrrolidone and 10-20 parts by weight of water, then adding 2-5 parts by weight of the surface-modified silica / alumina composite and 1-4 parts by weight of aminated polyvinyl alcohol, and ultrasonically dispersing for 10-20 minutes at a power of 100-200 W and a frequency of 20-30 kHz, then adding 6-8 parts by weight of ethyl methacrylate, 2-4 parts by weight of butyl acrylate and 0.05-0.15 parts by weight of ammonium persulfate, and reacting at 80-90°C under a nitrogen atmosphere for 5-8 hours to obtain an intermediate material; mixing 2-4 parts by weight of acrylic acid, 6-8 parts by weight of ethyl methacrylate, 1-4 parts by weight of butyl acrylate, 1-2 parts by weight of hydroxypropyl acrylate, 0.3-0.8 parts by weight of methacrylamide and 0.1-0.3 parts by weight of ammonium persulfate, and stirring at 75-80°C and 100-200 rpm for 20-40 minutes, then adding 10-30 parts by weight of the intermediate material and continuing to stir for 1-3 hours, and then cooling to room temperature, and adjusting the pH to neutral to obtain an aqueous resin emulsion.

[0020] Preferably, the method for preparing the adhesion promoter comprises the following steps:

[0021] Mixing 20-35 parts by weight of an aqueous phytic acid solution and 2-5 parts by weight of glycidyl propyl acrylate, then adding 0.1-0.3 parts by weight of tetrabutylammonium bromide and 0.03-0.05 parts by weight of hydroquinone, and heating to react, extracting, and then distilling under reduced pressure to obtain an alkenyl-grafted phytic acid; mixing 8-12 parts by weight of hydroxypropyl acrylate, 1-3 parts by weight of isomeric tridecanol polyoxyethylene ether and 1-2 parts by weight of γ-aminopropyl triethoxysilane, then adding 3-6 parts by weight of the alkenyl-grafted phytic acid under a nitrogen atmosphere and stirring, then adding 0.5-0.8 parts by weight of water and continuing to stir, and then cooling to obtain the adhesion promoter.

[0022] The application uses hydroxypropyl acrylate, isomeric tridecanol polyoxyethylene ether, gamma-aminopropyl triethoxysilane and alkenyl grafted phytic acid as raw materials to prepare an adhesion promoter, which can effectively improve the adhesion performance of water-based paint. During the whole process, the components form a complex three-dimensional network structure through chemical bonding and interaction, so that the adhesion promoter can not only be firmly attached to the surface of the substrate, but also be closely combined with the film-forming resin, thereby further improving the adhesion performance of the water-based paint. Among them, the phosphate groups of the alkenyl grafted phytic acid can form a firm coordination bond or covalent bond with the hydroxyl groups or oxide layer on the surface of the substrate to enhance the adhesion, and the unsaturated double bond can participate in the crosslinking reaction to improve the durability of the coating; the silicon-oxygen bond generated by the gamma-aminopropyl triethoxysilane has a hydrogen bond effect with the carboxyl / hydroxyl groups in the film-forming resin, further enhancing the adhesion and compatibility.

[0023] Further, the preparation method of the adhesion promoter comprises the following steps:

[0024] Mix 20-35 parts by weight of 15-30 wt% phytic acid aqueous solution with 2-5 parts by weight of propylene glycol acrylate, then add 0.1-0.3 parts by weight of tetrabutylammonium bromide and 0.03-0.05 parts by weight of hydroquinone, and react at 85-90°C and 200-400 rpm for 1-3 h, extract with ethyl acetate, then recover ethyl acetate by reduced pressure distillation to obtain alkenyl grafted phytic acid; mix 8-12 parts by weight of hydroxypropyl acrylate, 1-3 parts by weight of isomeric tridecanol polyoxyethylene ether and 1-2 parts by weight of gamma-aminopropyl triethoxysilane, add 3-6 parts by weight of alkenyl grafted phytic acid under the conditions of nitrogen atmosphere, 70-75°C and 200-400 rpm stirring, and stir for 4-6 h, then add 0.5-0.8 parts by weight of water and continue to stir for 1-2 h, and cool to room temperature to obtain the adhesion promoter.

[0025] Preferably, the water-based dispersant is one of dispersant EDAPLAN 490, dispersant EDAPLAN 516, dispersant EDAPLAN 397 or a mixture of two or more thereof; brand: Mingling, Germany.

[0026] Preferably, the water-based defoamer is one of defoamer BYK-016, defoamer BYK-012, defoamer BYK-011 or a mixture of two or more thereof; brand: BYK, Germany.

[0027] Preferably, the film-forming aid is one of ethylene glycol ethyl ether, ethylene glycol butyl ether, tripropylene glycol butyl ether or a mixture of two or more thereof.

[0028] The application also provides a preparation method of water-based printing paint, comprising the following steps:

[0029] The water-based printing paint is prepared by mixing the water-based resin emulsion, the adhesion promoter, the water-based dispersant and water according to the raw material formula, stirring at 30-40 DEG C and 400-500 rpm for 15-30 min, then adding the water-based defoaming agent and the film-forming aid and continuing to stir for 3-8 min, and cooling to room temperature.

[0030] The application further provides application of the water-based printing paint in digital inkjet printing.

[0031] Compared with the prior art, the application has the following advantages and beneficial effects:

[0032] 1. The application provides a water-based printing paint and a preparation method thereof, which adds specific water-based resin emulsion and adhesion promoter in the raw material formula, wherein the water-based resin emulsion is prepared from surface-modified silicon dioxide / aluminum oxide composite, aminated polyvinyl alcohol and acrylic monomer, and the adhesion promoter is prepared from hydroxypropyl acrylate, isomeric tridecanol polyoxyethylene ether, gamma-aminopropyl triethoxysilane and alkenyl grafted phytic acid, so that the adhesion and wear resistance of the paint are further improved, and the paint has the advantages of green environmental protection and good printing effect.

[0033] 2. The water-based resin emulsion prepared by the application has good adhesion and significantly improved wear resistance through synergistic effect of multiple mechanisms. Sodium dodecyl sulfate and polyvinylpyrrolidone are added to play the role of dispersant and stabilizer, so that uniform dispersion of components in the water phase is ensured, and particle agglomeration is avoided. Ammonium persulfate as an initiator promotes the polymerization reaction of the acrylate monomer to generate the water-based resin emulsion with excellent performance. The emulsion introduces the surface-modified silicon dioxide / aluminum oxide composite to provide the role of hard filler and enhance the hardness and wear resistance of the coating, and introduces the aminated polyvinyl alcohol to enhance the overall structural stability and flexibility of the coating through chemical bonding and crosslinking. The water-based resin emulsion realizes the dual improvement of the adhesion and wear resistance of the paint by simultaneously introducing the surface-modified silicon dioxide / aluminum oxide composite and the aminated polyvinyl alcohol, combining the miniemulsion polymerization method and the formation of the crosslinking network, and significantly prolongs the service life of the product.

[0034] 3. The adhesion promoter used in the application is prepared from hydroxypropyl acrylate, isomeric tridecanol polyoxyethylene ether, gamma-aminopropyl triethoxysilane and alkenyl grafted phytic acid, and can effectively improve the adhesion of the water-based printing paint. During the whole process, the components form a complex three-dimensional network structure through chemical bonding and interaction, so that the adhesion promoter can not only be firmly attached to the surface of the substrate, but also be closely combined with the film-forming resin, thereby further improving the adhesion of the water-based paint. DETAILED DESCRIPTION

[0035] The technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are only part 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 of ordinary skill in the art without creative work fall within the protection scope of the present application.

[0036] Embodiment 1

[0037] The present embodiment provides a water-based printing paint, which comprises the following raw materials in parts by weight:

[0038] 60 parts by weight of a water-based resin emulsion, 1.5 parts by weight of an adhesion promoter, 1 part by weight of a water-based dispersant, 0.5 parts by weight of a water-based defoamer, 2 parts by weight of a film-forming aid, and 35 parts by weight of water. The water-based dispersant is dispersant EDAPLAN® 490; the water-based defoamer is defoamer BYK-016; and the film-forming aid is ethylene glycol ethyl ether.

[0039] The preparation method of the water-based resin emulsion comprises the following steps:

[0040] 6.5 parts by weight of polyvinyl alcohol, 3.5 parts by weight of epichlorohydrin, and 90 parts by weight of 0.37wt% hydrochloric acid are mixed, stirred at 68°C and 150rpm for 50min, centrifuged, and dried to obtain an intermediate; 4 parts by weight of the intermediate, 0.05 parts by weight of tetrabutylammonium bromide, and 50 parts by weight of 0.5wt% ammonia water are mixed, then 20 parts by weight of ethylenediamine is added, and stirred at 68°C and 150rpm for 3h, centrifuged, and dried to obtain aminated polyvinyl alcohol; wherein the viscosity (25°C) of the polyvinyl alcohol is 20-30mPa.s, and the alcoholysis degree is 95-90%;

[0041] 10 parts by weight of tetraethyl orthosilicate, 25 parts by weight of aluminum nitrate, and 120 parts by weight of anhydrous ethanol are mixed to obtain a mixed solution, the mixed solution is added to 180 parts by weight of 16.5wt% ammonia water under the condition of stirring at 35°C and 600rpm for 7h, filtered, dried, and then calcined at 500°C for 2.5h to obtain a silica / alumina composite; 6 parts by weight of the silica / alumina composite and 50 parts by weight of water are mixed and stirred at room temperature and 600rpm for 0.5h, then 1.2 parts by weight of 3-acrylamidopropyl tris(trimethylsiloxy)silane is added, the temperature is raised to 86°C and the stirring is continued for 12h, the temperature is cooled to room temperature, filtered, and dried to obtain a surface-modified silica / alumina composite;

[0042] Mix 0.3 parts by weight of sodium lauryl sulfate, 0.1 parts by weight of polyvinylpyrrolidone with 15 parts by weight of water, then add 3.5 parts by weight of surface modified silica / alumina composite and 2.5 parts by weight of aminated polyvinyl alcohol, ultrasonically disperse for 15 min, the ultrasonic power is 150 W, the frequency is 20 kHz, then add 7 parts by weight of ethyl methacrylate, 3 parts by weight of butyl acrylate and 0.1 parts by weight of ammonium persulfate, react at 85°C under nitrogen atmosphere for 6h, to obtain an intermediate material; wherein the average molecular weight of polyvinylpyrrolidone is 10000;

[0043] Mix 3 parts by weight of acrylic acid, 7 parts by weight of ethyl methacrylate, 2.5 parts by weight of butyl acrylate, 1.5 parts by weight of hydroxypropyl acrylate, 0.5 parts by weight of methacrylamide and 0.2 parts by weight of ammonium persulfate, stir at 78°C, 150 rpm for 30 min, then add 20 parts by weight of the intermediate material and continue stirring for 2h, cool to room temperature, adjust the pH to neutral, to obtain an aqueous resin emulsion.

[0044] The preparation method of the adhesion promoter comprises the following steps:

[0045] Mix 30 parts by weight of 20wt% phytic acid aqueous solution with 3.5 parts by weight of glycidyl propyl acrylate, then add 0.2 parts by weight of tetrabutylammonium bromide, 0.04 parts by weight of hydroquinone, react at 86°C, 300 rpm for 2h, extract with ethyl acetate, then recover ethyl acetate by reduced pressure distillation, to obtain an alkenyl grafted phytic acid; Mix 10 parts by weight of hydroxypropyl acrylate, 2 parts by weight of isomeric tridecanol polyoxyethylene ether E1340, 1.2 parts by weight of γ-aminopropyl triethoxysilane, under the conditions of nitrogen atmosphere, 72°C, 300 rpm stirring, add 5 parts by weight of alkenyl grafted phytic acid and stir for 5h, then add 0.6 parts by weight of water and continue stirring for 1.5h, cool to room temperature, to obtain an adhesion promoter.

[0046] The present embodiment provides a preparation method of an aqueous printing paint, comprising the following steps:

[0047] Mix the aqueous resin emulsion, the adhesion promoter, the aqueous dispersant and water according to the raw material formula, stir at 35°C, 450 rpm for 20 min, then add the aqueous defoaming agent and the film-forming aid and continue stirring for 5 min, cool to room temperature, to obtain the aqueous printing paint.

[0048] Example 2

[0049] The present embodiment provides an aqueous printing paint, comprising the following parts by weight of raw material composition:

[0050] 55 parts by weight of the water-based resin emulsion, 1 part by weight of the adhesion promoter, 0.7 parts by weight of the water-based dispersant, 0.3 parts by weight of the water-based defoamer, 1 part by weight of the film-forming aid, and 30 parts by weight of water. The water-based dispersant is dispersant EDAPLAN® 490; the water-based defoamer is defoamer BYK-016; and the film-forming aid is ethylene glycol ethyl ether.

[0051] The preparation method of the water-based resin emulsion is the same as that in Example 1.

[0052] The preparation method of the adhesion promoter is the same as that in Example 1.

[0053] The present example provides a preparation method of a water-based printing paint, comprising the following steps:

[0054] The water-based resin emulsion, the adhesion promoter, the water-based dispersant, and water are mixed according to the raw material formula, stirred at 30°C and 400 rpm for 30 min, then the water-based defoamer and the film-forming aid are added and stirred for 8 min, and then cooled to room temperature to obtain the water-based printing paint.

[0055] Example 3

[0056] The present example provides a water-based printing paint, comprising the following raw material components by weight:

[0057] 65 parts by weight of the water-based resin emulsion, 2 parts by weight of the adhesion promoter, 1.2 parts by weight of the water-based dispersant, 0.6 parts by weight of the water-based defoamer, 3 parts by weight of the film-forming aid, and 40 parts by weight of water. The water-based dispersant is dispersant EDAPLAN® 490; the water-based defoamer is defoamer BYK-016; and the film-forming aid is ethylene glycol ethyl ether.

[0058] The preparation method of the water-based resin emulsion is the same as that in Example 1.

[0059] The preparation method of the adhesion promoter is the same as that in Example 1.

[0060] The present example provides a preparation method of a water-based printing paint, comprising the following steps:

[0061] The water-based resin emulsion, the adhesion promoter, the water-based dispersant, and water are mixed according to the raw material formula, stirred at 40°C and 500 rpm for 15 min, then the water-based defoamer and the film-forming aid are added and stirred for 3 min, and then cooled to room temperature to obtain the water-based printing paint.

[0062] Comparative Example 1

[0063] The difference between the present comparative example and Example 1 is that the preparation method of the water-based resin emulsion is different, specifically as follows: the preparation method of the water-based resin emulsion comprises the following steps:

[0064] A mixture of 10 parts by weight of tetraethyl orthosilicate, 25 parts by weight of aluminum nitrate and 120 parts by weight of anhydrous ethanol was obtained, and the mixture was added to 180 parts by weight of 16.5 wt% ammonia water at 35°C under stirring at 600 rpm for 7h, filtered, dried, and then calcined at 500°C for 2.5h to obtain a silica / alumina composite; 6 parts by weight of the silica / alumina composite was mixed with 50 parts by weight of water under stirring at 600 rpm at room temperature for 0.5h, and then 1.2 parts by weight of 3-acrylamidopropyl tris(trimethylsiloxy)silane was added, and the temperature was raised to 86°C for further stirring for 12h, and then the temperature was lowered to room temperature, filtered, and dried to obtain a surface-modified silica / alumina composite;

[0065] A mixture of 0.3 parts by weight of sodium dodecyl sulfate, 0.1 parts by weight of polyvinylpyrrolidone and 15 parts by weight of water was obtained, and then 3.5 parts by weight of the surface-modified silica / alumina composite was ultrasonically dispersed for 15 min at a power of 150 W and a frequency of 20 kHz, and then 7 parts by weight of ethyl methacrylate, 3 parts by weight of butyl acrylate and 0.1 parts by weight of ammonium persulfate were added, and the reaction was carried out at 85°C under a nitrogen atmosphere for 6h to obtain an intermediate material; wherein the average molecular weight of the polyvinylpyrrolidone was 10000;

[0066] A mixture of 3 parts by weight of acrylic acid, 7 parts by weight of ethyl methacrylate, 2.5 parts by weight of butyl acrylate, 1.5 parts by weight of hydroxypropyl acrylate, 0.5 parts by weight of methacrylamide and 0.2 parts by weight of ammonium persulfate was obtained, and then the mixture was stirred at 78°C at 150 rpm for 30 min, and then 20 parts by weight of the intermediate material was added for further stirring for 2h, and then the temperature was lowered to room temperature, and the pH was adjusted to neutral to obtain an aqueous resin emulsion.

[0067] Comparative Example 2

[0068] The difference between the present comparative example and Example 1 is that the preparation method of the aqueous resin emulsion is different, and the preparation method of the aqueous resin emulsion comprises the following steps:

[0069] A mixture of 6.5 parts by weight of polyvinyl alcohol, 3.5 parts by weight of epichlorohydrin and 90 parts by weight of 0.37 wt% hydrochloric acid was obtained, and then the mixture was stirred at 68°C at 150 rpm for 50 min, centrifuged, and dried to obtain an intermediate; a mixture of 4 parts by weight of the intermediate, 0.05 parts by weight of tetrabutylammonium bromide and 50 parts by weight of 0.5 wt% ammonia water was obtained, and then 20 parts by weight of ethylenediamine was added, and the mixture was stirred at 68°C at 150 rpm for 3h, centrifuged, and dried to obtain an aminated polyvinyl alcohol; wherein the viscosity (25°C) of the polyvinyl alcohol was 20-30 mPa.s, and the alcoholysis degree was 95-90%;

[0070] Mix 0.3 parts by weight of sodium dodecyl sulfate, 0.1 parts by weight of polyvinylpyrrolidone with 15 parts by weight of water, then add 2.5 parts by weight of aminated polyvinyl alcohol and ultrasonically disperse for 15 min, the ultrasonic power is 150 W, the frequency is 20 kHz, then add 7 parts by weight of ethyl methacrylate, 3 parts by weight of butyl acrylate and 0.1 parts by weight of ammonium persulfate, react for 6 h at 85℃ under nitrogen atmosphere, to obtain intermediate material; wherein the average molecular weight of polyvinylpyrrolidone is 10000;

[0071] Mix 3 parts by weight of acrylic acid, 7 parts by weight of ethyl methacrylate, 2.5 parts by weight of butyl acrylate, 1.5 parts by weight of hydroxypropyl acrylate, 0.5 parts by weight of methacrylamide and 0.2 parts by weight of ammonium persulfate, stir for 30 min at 78℃, 150 rpm, then add 20 parts by weight of intermediate material and continue to stir for 2 h, cool to room temperature, adjust the pH to neutral, to obtain an aqueous resin emulsion.

[0072] Comparative Example 3

[0073] The difference between this comparative example and Example 1 is that the preparation method of the aqueous resin emulsion is different, specifically as follows: the preparation method of the aqueous resin emulsion comprises the following steps:

[0074] Mix 10 parts by weight of tetraethyl orthosilicate, 25 parts by weight of aluminum nitrate with 120 parts by weight of anhydrous ethanol to obtain a mixed solution, add the mixed solution to 180 parts by weight of 16.5wt% ammonia water under stirring conditions of 35℃, 600 rpm for 7 h, filter, dry, and then calcine at 500℃ for 2.5 h to obtain a silica / alumina composite;

[0075] Mix 0.3 parts by weight of sodium dodecyl sulfate, 0.1 parts by weight of polyvinylpyrrolidone with 15 parts by weight of water, then add 3.5 parts by weight of silica / alumina composite and 2.5 parts by weight of polyvinyl alcohol and ultrasonically disperse for 15 min, the ultrasonic power is 150 W, the frequency is 20 kHz, then add 7 parts by weight of ethyl methacrylate, 3 parts by weight of butyl acrylate and 0.1 parts by weight of ammonium persulfate, react for 6 h at 85℃ under nitrogen atmosphere, to obtain intermediate material; wherein the average molecular weight of polyvinylpyrrolidone is 10000;

[0076] Mix 3 parts by weight of acrylic acid, 7 parts by weight of ethyl methacrylate, 2.5 parts by weight of butyl acrylate, 1.5 parts by weight of hydroxypropyl acrylate, 0.5 parts by weight of methacrylamide and 0.2 parts by weight of ammonium persulfate, stir for 30 min at 78℃, 150 rpm, then add 20 parts by weight of intermediate material and continue to stir for 2 h, cool to room temperature, adjust the pH to neutral, to obtain an aqueous resin emulsion.

[0077] Comparative Example 4

[0078] The difference between this comparative example and Example 1 is that the preparation method of the aqueous resin emulsion is different, specifically as follows: the preparation method of the aqueous resin emulsion comprises the following steps:

[0079] Mix 6.5 parts by weight of polyvinyl alcohol, 3.5 parts by weight of epichlorohydrin and 90 parts by weight of 0.37wt% hydrochloric acid, stir at 68°C and 150 rpm for 50 min, centrifuge, dry to obtain an intermediate; mix 4 parts by weight of the intermediate, 0.05 parts by weight of tetrabutylammonium bromide and 50 parts by weight of 0.5wt% ammonia water, then add 20 parts by weight of ethylenediamine, stir at 68°C and 150 rpm for 3h, centrifuge, dry to obtain aminated polyvinyl alcohol; wherein the viscosity (25°C) of the polyvinyl alcohol is 20-30 mPa.s and the alcoholysis degree is 95-90%;

[0080] Mix 6 parts by weight of silica and 50 parts by weight of water, stir at room temperature and 600 rpm for 0.5h, then add 1.2 parts by weight of 3-acrylamidopropyl tris(trimethylsiloxy)silane, continue to stir at 86°C for 12h, cool to room temperature, filter and dry to obtain surface-modified silica; wherein the average particle size of the silica is 50-100 nm;

[0081] Mix 0.3 parts by weight of sodium dodecyl sulfate, 0.1 parts by weight of polyvinylpyrrolidone and 15 parts by weight of water, then add 3.5 parts by weight of surface-modified silica and 2.5 parts by weight of aminated polyvinyl alcohol and ultrasonically disperse for 15 min, the ultrasonic power is 150 W and the frequency is 20 kHz, then add 7 parts by weight of ethyl methacrylate, 3 parts by weight of butyl acrylate and 0.1 parts by weight of ammonium persulfate, react at 85°C under a nitrogen atmosphere for 6h to obtain an intermediate material; wherein the average molecular weight of the polyvinylpyrrolidone is 10000;

[0082] Mix 3 parts by weight of acrylic acid, 7 parts by weight of ethyl methacrylate, 2.5 parts by weight of butyl acrylate, 1.5 parts by weight of hydroxypropyl acrylate, 0.5 parts by weight of methacrylamide and 0.2 parts by weight of ammonium persulfate, stir at 78°C and 150 rpm for 30 min, then add 20 parts by weight of the intermediate material and continue to stir for 2h, cool to room temperature, adjust the pH to neutral to obtain an aqueous resin emulsion.

[0083] Comparative Example 5

[0084] The difference between this comparative example and Example 1 is that the self-made adhesion promoter in Example 1 is replaced by a commercially available adhesion promoter Silok®6208 (brand: Silok).

[0085] Comparative Example 6

[0086] The difference between the present comparative example and example 1 is that the preparation method of the adhesion promoter is different, specifically as follows: the preparation method of the adhesion promoter comprises the following steps:

[0087] 10 parts by weight of hydroxypropyl acrylate, 2 parts by weight of isomeric tridecanol polyoxyethylene ether E1340, 1.2 parts by weight of γ-aminopropyl triethoxysilane are mixed, 5 parts by weight of polyphosphoric acid (85% P2O5) is added under the condition of nitrogen atmosphere, 72°C, 300rpm stirring for 5h, then 0.6 parts by weight of water is added and continue to stir for 1.5h, and then cooled to room temperature to obtain the adhesion promoter.

[0088] Performance test

[0089] The water-based printing paint obtained in examples 1-3 and comparative examples 1-6 of the present application is uniformly coated on the surface of a polypropylene substrate, and after curing to form a coating layer (thickness of 40μm), the test is carried out. Among them, the adhesion test refers to the standard GB / T 9286-2021 (0-5 level, 5 level is the worst), the wear resistance test refers to the standard GB / T 1768-2006, and the VOC content test refers to the standard GB / T 23986-2009. The results are shown in Table 1.

[0090] Table 1: Performance test results of water-based printing paint

[0091]

[0092] From the above performance test results, it can be seen that the water-based printing paint prepared in examples 1-3 has good adhesion performance and wear resistance, and the VOC content is low, especially the water-based printing paint of example 1 has the most outstanding comprehensive performance, because the specific water-based resin emulsion and adhesion promoter are used in the present application, which significantly improves the adhesion performance and wear resistance of the water-based printing paint.

[0093] In comparison, comparative examples 1-6 do not use the necessary technical solutions, resulting in a significant difference in the corresponding performance test compared with examples 1-3. In comparative example 1-4, a specific water-based resin emulsion is not used, and in comparative examples 5-6, a self-made adhesion promoter is not used. As can be seen from the results, it leads to a decrease in the adhesion performance and wear resistance of the water-based printing paint. The above experimental results further prove the importance of the technical solutions defined in the present application to its technical effects.

[0094] The above is the preferred embodiment of the present application. It should be noted that for ordinary skilled persons in the technical field, without departing from the principles of the present application, a number of improvements and refinements can be made, which should also be considered as the protection scope of the present application.

Claims

1. 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obtain an aqueous resin emulsion.

2. The aqueous print coating according to claim 1, characterized in that The method for preparing the adhesion promoter comprises the following steps: Mix 20-35 parts by weight of a 15-30 wt% aqueous phytic acid solution with 2-5 parts by weight of glycidyl propyl acrylate, then add 0.1-0.3 parts by weight of tetrabutylammonium bromide and 0.03-0.05 parts by weight of hydroquinone, react at 85-90°C and 200-400 rpm for 1-3 h, extract with ethyl acetate, then recover the ethyl acetate by distillation under reduced pressure to obtain an alkenyl-grafted phytic acid; mix 8-12 parts by weight of hydroxypropyl acrylate, 1-3 parts by weight of isomeric tridecyl polyoxyethylene ether and 1-2 parts by weight of γ-aminopropyl triethoxysilane, then add 3-6 parts by weight of the alkenyl-grafted phytic acid under stirring at 70-75°C and 200-400 rpm for 4-6 h, then add 0.5-0.8 parts by weight of water and continue stirring for 1-2 h, and cool to room temperature to obtain the adhesion promoter.

3. The aqueous print coating according to claim 1, characterized in that The method for preparing the aqueous resin emulsion comprises the following steps: Mix 5-8 parts by weight of polyvinyl alcohol, 2-5 parts by weight of epichlorohydrin with 80-100 parts by weight of 0.2-0.5 wt% hydrochloric acid, stir at 65-70°C and 100-200 rpm for 40-60 min, centrifuge, and dry to obtain an intermediate; mix 3-5 parts by weight of the intermediate, 0.03-0.06 parts by weight of tetrabutylammonium bromide with 40-60 parts by weight of 0.3-0.6 wt% ammonia water, then add 15-25 parts by weight of ethylenediamine, stir at 65-70°C and 100-200 rpm for 2-4 h, centrifuge, and dry to obtain aminated polyvinyl alcohol; Mixing 8-12 parts by weight of ethyl orthosilicate, 20-30 parts by weight of aluminum nitrate and 100-150 parts by weight of anhydrous ethanol to obtain a mixed solution, adding the mixed solution into 150-200 parts by weight of 15-18 wt% ammonia water under the condition of 30-40℃ and 500-700 rpm stirring for 6-8 hours, filtering, drying, and then calcining at 450-550℃ for 2-4 hours to obtain a silica / alumina composite; mixing 5-7 parts by weight of the silica / alumina composite and 40-60 parts by weight of water under the condition of room temperature and 500-700 rpm stirring for 0.3-0.6 hours, then adding 1-1.5 parts by weight of 3-acrylamidopropyl tris(trimethylsiloxy) silane, and continuing to stir at 85-90℃ for 10-15 hours, cooling to room temperature, filtering, and drying to obtain a surface-modified silica / alumina composite; Mixing 0.2-0.5 parts by weight of sodium dodecyl sulfate, 0.08-0.12 parts by weight of polyvinylpyrrolidone and 10-20 parts by weight of water, then adding 2-5 parts by weight of the surface-modified silica / alumina composite and 1-4 parts by weight of aminated polyvinyl alcohol, and ultrasonic dispersing for 10-20 minutes with a power of 100-200 W and a frequency of 20-30 kHz, then adding 6-8 parts by weight of ethyl methacrylate, 2-4 parts by weight of butyl acrylate and 0.05-0.15 parts by weight of ammonium persulfate, and reacting at 80-90℃ under a nitrogen atmosphere for 5-8 hours to obtain an intermediate material; mixing 2-4 parts by weight of acrylic acid, 6-8 parts by weight of ethyl methacrylate, 1-4 parts by weight of butyl acrylate, 1-2 parts by weight of hydroxypropyl acrylate, 0.3-0.8 parts by weight of methacrylamide and 0.1-0.3 parts by weight of ammonium persulfate, and stirring at 75-80℃ and 100-200 rpm for 20-40 minutes, then adding 10-30 parts by weight of the intermediate material and continuing to stir for 1-3 hours, and cooling to room temperature to obtain a water-based resin emulsion with a neutral pH.

4. The aqueous print coating of claim 1, wherein, The water-based dispersant is one of dispersant EDAPLAN® 490, dispersant EDAPLAN® 516, dispersant EDAPLAN® 397 or a mixture of two or more thereof.

5. The aqueous print coating of claim 1, wherein, The water-based defoaming agent is one of defoaming agent BYK-016, defoaming agent BYK-012, defoaming agent BYK-011 or a mixture of two or more thereof.

6. The aqueous print coating of claim 1, wherein, The film-forming aid is one of ethylene glycol ethyl ether, ethylene glycol butyl ether, tripropylene glycol butyl ether or a mixture of two or more thereof.

7. The process for the preparation of an aqueous printing coating according to any one of claims 1 to 6, characterized in that The method comprises the following steps: Mixing the water-based resin emulsion, the adhesion promoter, the water-based dispersant and water according to the raw material formula, stirring at 30-40℃ and 400-500 rpm for 15-30 minutes, then adding the water-based defoaming agent and the film-forming aid and continuing to stir for 3-8 minutes, and cooling to room temperature to obtain the water-based printing paint.

8. Use of the water-based printing paint according to any one of claims 1-6 in digital inkjet printing.

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