CN115975485B - Water-based primer-topcoat coating - Google Patents
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Abstract
The invention discloses a water-based primer-topcoat coating, which comprises a paint component and a curing agent, wherein the paint component comprises epoxy acrylic acid aqueous dispersion, antirust pigment, coloring pigment, filler, anti-flash rust agent, hydrophobic agent, dispersing agent, defoaming agent, substrate wetting agent, anti-settling agent, hydrophilic cosolvent and water; wherein the epoxy acrylic acid aqueous dispersion is obtained by copolymerizing epoxy resin, vinyl monomer and organosilicon. In the water-based primer-topcoat coating, after double bonds in the organosilicon 1-hydroxy allyl trimethyl silane participate in acrylic ester copolymerization, free hydroxy groups are polymerized with hydroxy groups in acrylic ester and hydroxy groups in epoxy resin together with isocyanate, so that the hidden danger of weather resistance reduction caused by migration of anti-aging auxiliary agents in the coating can be avoided, and the wettability of the coating with a base material after curing can be improved. The coating obtained after the coating is coated by the coating disclosed by the invention has the purposes of corrosion resistance, rust resistance, light resistance and the like, has a long protection period and meets the coating requirements of vehicle parts.
Description
Technical Field
The invention relates to the field of coatings, in particular to a water-based primer-topcoat coating.
Background
The pressure of environmental protection promotes the vehicle coating to accelerate the water-based and solvent-free, however, the self-drying system with the water-based coating often has the problems of insufficient protective performance, strong cohesive force of the coating, excessively rapid decrease of adhesion after a long time, and the like; in addition, the water-based paint is generally higher in cost than a solvent-based system due to the limitation of raw materials and the state of the art, so that the application of the water-based paint in the field of vehicle coating is limited. Therefore, how to reduce the coating cost and meet the requirements of protecting and decorating the vehicle structural parts has prompted the generation of paint for coating the vehicle structural parts with the integrated bottom surface.
Although the aqueous epoxy coating system can realize good protective performance of the coating, the common epoxy system has defects in light resistance due to bisphenol A in the structure, which limits the application of the epoxy system as a coating finish, especially a vehicle finish, but the epoxy system has strong environmental corrosion resistance and is often the first choice system of self-drying vehicle primer.
The acrylic polyurethane coating not only has good decorative property after film formation, but also has excellent light resistance, and simultaneously has broad-spectrum adaptability to a substrate, and can be suitable for plastics such as ABS, PVC, HIPS, ASA, PMMA and various metals.
In view of the characteristics of acrylic acid and epoxy performance, if the corrosion resistance and the light resistance of epoxy and acrylic acid can be considered in a film forming system, single-coating of vehicle parts can be realized, and the coating cost caused by the water-based coating is reduced.
However, in most cases, the compatibility of epoxy systems with acrylic systems is not ideal due to the difference in hydrogen bond values, and particularly in aqueous dispersion systems, the surface tension of acrylic aqueous dispersions or emulsions is higher than that of solvent-based systems, and compatibility cannot be achieved by cold-blending with typical epoxy systems.
Regarding the water-based primer-topcoat paint, chinese patent document CN102108250B (application No. 201110053774.7) discloses a water-based primer-topcoat anticorrosive paint and a preparation method thereof, wherein the water-based primer-topcoat anticorrosive paint comprises the following components in percentage by weight: 20-60% of waterborne polyurethane modified epoxy resin, 5-25% of deionized water, 0.5-5% of dispersing agent, 0.1-5% of defoaming agent, 0.1-5% of base material wetting agent, 10-40% of pigment and filler, 0.5-10% of pH regulator, 0.5-10% of thixotropic agent, 0.5-5% of film forming auxiliary agent, 1-5% of light stabilizer, 0.5-5% of flash corrosion inhibitor and 0-10% of salt spray resistant auxiliary agent. The waterborne polyurethane modified epoxy resin is prepared through the following steps: (1) 250kg of polyether glycol and 380kg of toluene diisocyanate are mixed and stirred, and the temperature is gradually increased to 100 ℃ for reaction for 1.5h; (2) 60kg of dimethylolbutyric acid and 20kg of trimethylolpropane are added, stirring is continued, and the reaction is carried out for 1 hour, thus obtaining a mixture; (3) 70kg of epoxy resin E-51 is dissolved in 120kg of acetone, and is added into the mixture dropwise for copolymerization for 1h, and a proper amount of acetone can be added in the reaction process to control the viscosity of the reaction system to 70 mPas; (4) Cooling to about 40 ℃, adding 60kg of triethylamine for neutralization, and reacting for 20min; (5) And dissolving the product in deionized water, adding 40kg of ethylenediamine for chain extension, and stirring at a speed of 1000 rpm for 30min to obtain the waterborne polyurethane modified epoxy resin.
Chinese patent document CN102627902B (application No. 201210075173.0) discloses a water-based acrylic acid modified epoxy primer-topcoat anti-corrosive baking paint and a preparation method thereof. The coating comprises the following raw material components in percentage by weight: 30-50% of aqueous acrylic modified epoxy emulsion, 3-7% of amino resin, 0.3-0.6% of amine regulator, 15-35% of water, 0-6% of cosolvent, 15-30% of pigment, 0.3-0.6% of anti-flash rust agent, 2-5% of salt spray resistant agent, 0.3-0.5% of wetting dispersant, 0.3-0.5% of defoaming agent, 0.3-0.5% of leveling agent and 0.4-1.1% of thickener. The aqueous acrylic acid modified epoxy emulsion is an aqueous dispersion emulsion prepared by directly mixing 25-35% of epichlorohydrin, 40-50% of bisphenol A, 5-15% of butyl acrylate, 5-15% of methyl methacrylate, 0.5-2% of vinylbenzenesulfonic acid dimethyl ethanolamine salt and 1-5% of styrene under the action of 0.1-0.5% of initiator through block polymerization and graft polymerization; the viscosity of the aqueous acrylic acid modified epoxy emulsion is 500-2000mPa.s, the weight solid content is 35-40%, and the pH value is 7-9.
Disclosure of Invention
The invention aims to solve the technical problem of providing an aqueous primer-topcoat coating with excellent comprehensive performance for coating vehicle metal parts and non-metal parts and a preparation method thereof.
The technical scheme for realizing the first purpose of the invention is that the water-based primer-topcoat integrated coating comprises a paint component and a curing agent, wherein the paint component comprises epoxy acrylic acid aqueous dispersion, antirust pigment, coloring pigment, filler, anti-flash rust agent, hydrophobing agent, dispersing agent, defoaming agent, substrate wetting agent, anti-settling agent, hydrophilic cosolvent and water; wherein the epoxy acrylic acid aqueous dispersion is obtained by copolymerizing epoxy resin, vinyl monomer and organosilicon.
The curing agent is aliphatic polyisocyanate, and the mass ratio of the paint component to the curing agent is 1-1.2:1.
Further, the preparation method of the epoxy acrylic acid aqueous dispersion comprises the following steps: adding epoxy resin into a reaction kettle, adding propylene glycol methyl ether into the reaction kettle, mixing, heating to 50-60 ℃, and stirring until the epoxy resin is completely dissolved; then heating to 100-120 ℃, beginning to drop vinyl monomer-organosilicon-initiator-propylene glycol methyl ether mixed solution, after finishing dropping for 2.5-3.5 hours, adding propylene glycol methyl ether-initiator mixed solution after heat preservation, continuing heat preservation for 4-5 hours, neutralizing with N, N-dimethylethanolamine to adjust the PH value, removing propylene glycol methyl ether by reduced pressure distillation, adding water for pre-dispersing and stirring uniformly to obtain the epoxy acrylic acid aqueous dispersion.
The epoxy resin accounts for 5% -15% of the total amount of solids in the epoxy acrylic acid aqueous dispersion.
The vinyl monomer is a composition of two or more of acrylic ester, methacrylic ester and styrene; the acrylic resin chain segment obtained by copolymerization is obtained by copolymerization of two or more than two of acrylic monomers, methacrylic monomers and styrene; the glass transition temperature of the acrylic resin chain segment is 50-70 ℃.
The organic silicon is 1-hydroxy allyl trimethyl silane; in the epoxy acrylic acid aqueous dispersion, the content of 1-hydroxy allyl trimethylsilane is 1 to 3wt% of the total solid.
The hydroxyl value of the epoxy acrylic acid aqueous dispersion is 1.3 to 1.5 percent based on the solid; the crosslinking curing reaction adopts the aqueous dispersion of aliphatic isocyanate to cure the hydroxyl groups in the film-forming resin at room temperature, and the NCO/OH ratio is 1.5-2.0: 1.
in the film-forming coating, the epoxy acrylic dispersion is used in an amount of 40 to 55 percent by weight of the total amount of solids in the paint component; the dosage of the antirust pigment is 10% -20% of the total solid in the paint component; the amount of the filler is 10% -20% of the total amount of solids in the paint component; the dosage of the flash rust inhibitor is 0.8% -1.0% of the total solid in the paint component; the dosage of the hydrophobizing agent is 0.5% -2% of the total amount of solids in the paint component; the dispersant accounts for 2% -25% of the total pigment and filler; the dosage of the base material wetting agent is 0.5% -2.0% of the total solid in the paint component; the dosage of the anti-settling agent is 0.5 to 4.0 percent of the total solid content in the paint component.
The technical scheme for realizing the second purpose of the invention is that the epoxy acrylic acid aqueous dispersion is prepared by the following method: adding epoxy resin into a reaction kettle, adding propylene glycol methyl ether into the reaction kettle, mixing, heating to 50-60 ℃, and stirring until the epoxy resin is completely dissolved; then heating to 100-120 ℃, beginning to drop vinyl monomer-organosilicon-initiator-propylene glycol methyl ether mixed solution, after finishing dropping for 2.5-3.5 hours, adding propylene glycol methyl ether-initiator mixed solution after heat preservation, continuing heat preservation for 4-5 hours, neutralizing with N, N-dimethylethanolamine to adjust the PH value, removing propylene glycol methyl ether by reduced pressure distillation, adding water for pre-dispersing and stirring uniformly to obtain the epoxy acrylic acid aqueous dispersion.
The epoxy resin accounts for 5% -15% of the total amount of solids in the epoxy acrylic acid aqueous dispersion.
The vinyl monomer is a composition of two or more of acrylic ester, methacrylic ester and styrene; the acrylic resin chain segment obtained by copolymerization is obtained by copolymerization of two or more than two of acrylic monomers, methacrylic monomers and styrene; the glass transition temperature of the acrylic resin chain segment is 50-70 ℃.
The organic silicon is 1-hydroxy allyl trimethyl silane; in the epoxy acrylic acid aqueous dispersion, the content of 1-hydroxy allyl trimethylsilane is 1 to 3wt% of the total solid.
The invention has the positive effects that: (1) In the water-based primer-topcoat coating, after double bonds in the organosilicon 1-hydroxy allyl trimethyl silane participate in acrylic ester copolymerization, free hydroxy groups are polymerized with hydroxy groups in acrylic ester and hydroxy groups in epoxy resin together with isocyanate, so that the hidden danger of weather resistance reduction caused by migration of anti-aging auxiliary agents in the coating can be avoided, and the wettability of the coating with a base material after curing can be improved.
(2) When the epoxy acrylic acid aqueous dispersion is prepared, an interpenetrating structure is formed between the acrylic acid and the epoxy resin in the acrylic acid-organosilicon copolymerization process, so that the mutual compatibility of acrylic ester and the epoxy resin is realized; the polymerization reaction has no hidden trouble of unstable and incomplete ring opening of the catalyst to the epoxy, and has no gel sequelae which may cause excessive molecular weight due to grafting.
After the epoxy acrylate with the interpenetrating structure is formed, hydroxyl on epoxy resin is easy to participate in isocyanate reaction together with hydroxyl (hydroxyl introduced by organosilicon chain unit and acrylic acid chain unit) on a hydroxyl resin chain segment at room temperature, and the formed film has good structural uniformity and complete protection (no break).
(3) The coating obtained after the coating is coated by the coating disclosed by the invention has the purposes of corrosion resistance, rust resistance, light resistance and the like, has a long protection period and meets the coating requirements of vehicle parts.
Detailed Description
The aqueous primer-topcoat coating disclosed by the invention is a two-component coating and comprises a paint component and a curing agent, wherein the curing agent is an aliphatic polyisocyanate aqueous dispersion, and the mass ratio of the paint component to the curing agent is 1-1.2:1.
The paint comprises epoxy acrylic acid aqueous dispersion, antirust pigment, coloring pigment, filler, composite flash rust inhibitor (passivation and complexation rust removal), water repellent, dispersing agent, defoamer, substrate wetting agent, sagging and sinking prevention auxiliary agent, hydrophilic cosolvent and water.
The preparation method of the epoxy acrylic acid aqueous dispersion comprises the following steps:
adding high molecular weight epoxy resin (609 epoxy resin) into a reaction kettle, adding propylene glycol methyl ether into the reaction kettle, mixing and heating to 50-60 ℃, and stirring until the epoxy resin is completely dissolved; then heating to 100-120 ℃, beginning to drop vinyl monomer-organosilicon-initiator-propylene glycol methyl ether mixed solution, after finishing dropping for 2.5-3.5 h, keeping the temperature for 1h, adding propylene glycol methyl ether-initiator mixed solution, continuing to keep the temperature for 4-5 h until the viscosity is qualified (the viscosity reaches 500-3000 Pa.s), neutralizing with N, N-dimethylethanolamine to adjust the PH value to be about 7, distilling under reduced pressure to remove propylene glycol methyl ether until the content is controlled within 10%, adding water for pre-dispersing and stirring to obtain epoxy acrylic acid aqueous dispersion, wherein the hydroxyl value is 1.3-1.5% (based on solid).
The epoxy resin accounts for 5% -15% of the total amount of solids in the epoxy acrylic acid aqueous dispersion.
The vinyl monomer is a composition of two or more of acrylic ester, methacrylic ester and styrene; correspondingly, the acrylic resin chain segment obtained by copolymerization is obtained by copolymerization of two or more than two of acrylic monomers, methacrylic monomers and styrene; the glass transition temperature of the acrylic resin chain segment is 50-70 ℃. The acrylic resin segments account for 45-55% of the total solids in the epoxy acrylic aqueous dispersion.
The organosilicon is 1-hydroxy allyl trimethyl silane containing difunctional groups (hydroxy and double bonds); in the prepared epoxy acrylic acid aqueous dispersion, the content of the 1-hydroxy allyl trimethyl silane is 1-3 wt% of the total solid.
The structural formula of the 1-hydroxy allyl trimethylsilane is as follows:
。
the initiator is a peroxide, such as benzoyl peroxide, dicumyl peroxide, etc., and benzoyl peroxide is selected in this embodiment.
In the film-forming coating, the epoxy acrylic dispersion is used in an amount of 40% to 55% by weight of the total solids in the paint component.
The antirust pigment is a composite zinc salt, and the dosage of the antirust pigment is 10-20% of the total solid content in the paint component.
The amount of the coloring pigment is 1 to 1.5% of the total amount of solids in the paint component.
The amount of the filler is 10% -20% of the total amount of solids in the paint component. The filler is one or more of mica powder, barium sulfate and talcum powder.
The compound flash rust inhibitor is a flash rust inhibitor combining non-chromium passivation and complexation rust removal, such as the flash rust inhibitor ZH-66 produced by Jiangsu Ten pine New material technology Co. The dosage (stock solution) of the composite flash rust inhibitor is 0.8-1.0% of the total solid content in the paint component.
The hydrophobing agent is organic silicon modified paraffin which does not affect recoating or repair, and the dosage of the hydrophobing agent is 0.5% -2% of the total solid in the paint component. For example, the hydrophobizing agent can be a hydrophobizing agent LW-102A produced by Nanjing Tianshi New Material technology Co.
The dispersant accounts for 2% -25% of the total pigment and filler, and the addition amount changes along with the change of the specific surface area of the pigment and filler; for example, the dispersant is byk190 from Pick chemical.
The defoamer may be PA311 defoamer of field chemistry.
The substrate wetting agent is long carbon chain (8-12 carbon) aminosilicone which is amino terminated and can be dispersed in water (with the help of a cosolvent), such as substrate wetting agent 4333 of Shanghai deep bamboo chemical auxiliary agent Co., ltd; the amount of the base material wetting agent is 0.5% -2.0% of the total amount of solids in the paint component.
The dosage of the anti-settling agent is 0.5% -4.0% of the total solid in the paint component; the use of aqueous polyurethane dispersions as anti-settling agents is, for example, TRK-928D, available from Heterolix New Material technologies Co.
The dosage of the hydrophilic cosolvent is 10-30% of the total solid content in the paint component; the hydrophilic cosolvent is one or more of propylene glycol butyl ether, isopropanol and propylene glycol methyl ether.
The curing agent is an aqueous aliphatic polyisocyanate dispersion, such as easaqa ™ L600 of Vencorex chemicals.
The preparation method of the paint component of the water-based primer-topcoat paint comprises the following steps: adding epoxy acrylic acid aqueous dispersion, a dispersing agent, a defoaming agent, deionized water and a small amount of hydrophilic cosolvent according to a metering ratio (the mass percent is the same as below), stirring and mixing uniformly in a mixing tank with stirring, then sequentially adding a composite zinc salt, a coloring pigment and a filler according to the metering ratio, dispersing at a high speed for half an hour, grinding and dispersing by a sand mill until fineness meets film forming requirements, and then adding auxiliary film forming materials such as a substrate wetting agent, a composite anti-flash rust agent, a hydrophobic agent and the like, and stirring uniformly to obtain the paint component of the water-based primer-topcoat material.
Specific examples are as follows:
(examples 1 to 5, epoxy acrylic aqueous dispersion)
According to the above-described method for producing an acrylic acid aqueous dispersion, the amounts of the acrylic acid aqueous dispersion raw materials of examples 1 to 5 are as follows:
(examples 6 to 11, paint component of aqueous primer-topcoat composition)
The paint components of the aqueous primer-topcoat compositions of examples 6 to 11 were composed as follows:
test example
The paint components of the examples 6 to 11 are ground to a fineness of below 25 mu m, respectively mixed and stirred with Easaqua ™ L600, and after coating, respectively crosslinked and cured to obtain a coating film; the mass ratio of the paint component to Easaqua ™ L600 is 1-1.2:1.
The properties of the coating film obtained after curing the paint components of each example were as follows (detection standard—corresponding national standard or industry standard):
from the results, the coating obtained after the coating is formed into a film has good salt spray resistance and light resistance; has excellent mechanical performance and good adhesion to various metals (such as zinc, iron and aluminum alloy) and various plastics (such as ABS, PVC, HIPS, ASA, PMMA).
Claims (3)
1. An aqueous primer-topcoat coating comprising a paint component and a curing agent, characterized in that: the paint comprises epoxy acrylic acid aqueous dispersion, antirust pigment, coloring pigment, filler, anti-flash rust agent, hydrophobic agent, dispersing agent, defoamer, substrate wetting agent, anti-settling agent, hydrophilic cosolvent and water;
in the film-forming coating, the epoxy acrylic dispersion is used in an amount of 40 to 55 percent by weight of the total amount of solids in the paint component; the dosage of the antirust pigment is 10% -20% of the total solid in the paint component; the amount of the filler is 10% -20% of the total amount of solids in the paint component; the dosage of the flash rust inhibitor is 0.8% -1.0% of the total solid in the paint component; the dosage of the hydrophobizing agent is 0.5% -2% of the total amount of solids in the paint component; the dispersant accounts for 2% -25% of the total pigment and filler; the dosage of the base material wetting agent is 0.5% -2.0% of the total solid in the paint component; the dosage of the anti-settling agent is 0.5 to 4.0 percent of the total solid in the paint component;
the curing agent is aliphatic polyisocyanate, and the mass ratio of the paint component to the curing agent is 1-1.2:1;
wherein the epoxy acrylic acid aqueous dispersion is obtained by copolymerizing epoxy resin, vinyl monomer and organosilicon;
the preparation method of the epoxy acrylic acid aqueous dispersion comprises the following steps: adding epoxy resin into a reaction kettle, adding propylene glycol methyl ether into the reaction kettle, mixing, heating to 50-60 ℃, and stirring until the epoxy resin is completely dissolved; then heating to 100-120 ℃, beginning to dropwise add vinyl monomer-organosilicon-initiator-propylene glycol methyl ether mixed solution, after 2.5-3.5 h of dropwise adding, keeping the temperature, adding propylene glycol methyl ether-initiator mixed solution, keeping the temperature for 4-5 h, neutralizing with N, N-dimethylethanolamine to adjust the pH value, removing propylene glycol methyl ether by reduced pressure distillation, adding water for pre-dispersing, and stirring uniformly to obtain epoxy acrylic acid aqueous dispersion;
the epoxy resin accounts for 5% -15% of the total amount of solids in the epoxy acrylic acid aqueous dispersion;
the vinyl monomer is a composition of two or more of acrylic ester, methacrylic ester and styrene; the acrylic resin chain segment obtained by copolymerization is obtained by copolymerization of two or more than two of acrylic monomers, methacrylic monomers and styrene; the glass transition temperature of the acrylic resin chain segment is 50-70 ℃;
the organic silicon is 1-hydroxy allyl trimethyl silane; in the epoxy acrylic acid aqueous dispersion, the content of 1-hydroxy allyl trimethylsilane is 1 to 3wt% of the total solid.
2. The aqueous primer-topcoat composition according to claim 1, wherein: the hydroxyl value of the epoxy acrylic acid aqueous dispersion is 1.3 to 1.5 percent based on the solid; the crosslinking curing reaction adopts the aqueous dispersion of aliphatic isocyanate to cure the hydroxyl groups in the film-forming resin at room temperature, and the NCO/OH ratio is 1.5-2.0: 1.
3. an epoxy acrylic acid aqueous dispersion is characterized by being prepared by the following method: adding epoxy resin into a reaction kettle, adding propylene glycol methyl ether into the reaction kettle, mixing, heating to 50-60 ℃, and stirring until the epoxy resin is completely dissolved; then heating to 100-120 ℃, beginning to dropwise add vinyl monomer-organosilicon-initiator-propylene glycol methyl ether mixed solution, after 2.5-3.5 h of dropwise adding, keeping the temperature, adding propylene glycol methyl ether-initiator mixed solution, keeping the temperature for 4-5 h, neutralizing with N, N-dimethylethanolamine to adjust the pH value, removing propylene glycol methyl ether by reduced pressure distillation, adding water for pre-dispersing, and stirring uniformly to obtain epoxy acrylic acid aqueous dispersion;
the epoxy resin accounts for 5% -15% of the total amount of solids in the epoxy acrylic acid aqueous dispersion;
the vinyl monomer is a composition of two or more of acrylic ester, methacrylic ester and styrene; the acrylic resin chain segment obtained by copolymerization is obtained by copolymerization of two or more than two of acrylic monomers, methacrylic monomers and styrene; the glass transition temperature of the acrylic resin chain segment is 50-70 ℃;
the organic silicon is 1-hydroxy allyl trimethyl silane; in the epoxy acrylic acid aqueous dispersion, the content of 1-hydroxy allyl trimethylsilane is 1 to 3wt% of the total solid.
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