CN116426186A - Water-based acrylic three-proofing paint and preparation method thereof - Google Patents

Water-based acrylic three-proofing paint and preparation method thereof Download PDF

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CN116426186A
CN116426186A CN202310704635.9A CN202310704635A CN116426186A CN 116426186 A CN116426186 A CN 116426186A CN 202310704635 A CN202310704635 A CN 202310704635A CN 116426186 A CN116426186 A CN 116426186A
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aqueous acrylic
acrylic resin
water
proofing paint
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钟来富
刘福春
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Institute of Corrosion Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
    • C09D133/04—Homopolymers or copolymers of esters
    • C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
    • C09D133/062—Copolymers with monomers not covered by C09D133/06
    • C09D133/066—Copolymers with monomers not covered by C09D133/06 containing -OH groups
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F212/02—Monomers containing only one unsaturated aliphatic radical
    • C08F212/04—Monomers containing only one unsaturated aliphatic radical containing one ring
    • C08F212/06—Hydrocarbons
    • C08F212/08—Styrene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/14—Methyl esters, e.g. methyl (meth)acrylate
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10—Esters
    • C08F220/12—Esters of monohydric alcohols or phenols
    • C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
    • C09D125/02—Homopolymers or copolymers of hydrocarbons
    • C09D125/04—Homopolymers or copolymers of styrene
    • C09D125/08—Copolymers of styrene
    • C09D125/14—Copolymers of styrene with unsaturated esters
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08—Anti-corrosive paints

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
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Abstract

The application discloses a water-based acrylic three-proofing paint which comprises the following components in parts by weight: 70-90 parts of aqueous acrylic resin, 6-10 parts of film forming auxiliary agent, 0.2-0.4 part of defoamer, 0.2-0.4 part of surfactant, 0.2-1.0 part of adhesion promoter and 0.05-0.2 part of fluorescent indicator; the glass transition temperature of the aqueous acrylic resin is 30-40 ℃. The application also discloses a preparation method of the water-based acrylic three-proofing paint. The water-based acrylic resin with specific glass transition temperature (Tg) is used as a main raw material, so that the purposes of improving the solid content and the mechanical property of the water-based three-proofing paint and reducing the cost are achieved.

Description

Water-based acrylic three-proofing paint and preparation method thereof
Technical Field
The invention relates to the technical field of coatings, in particular to a water-based acrylic three-proofing paint and a preparation method thereof.
Background
With the development of 5G technology communication technology, electronic products are gradually turned to miniaturization, integration and multifunctionality. In the actual use process of the electronic product, severe and complex service environments such as humidity, salt fog, high dust, high heat, low temperature, oil mist, vibration and the like can be met, and the circuit board and components thereof (integrated circuits, resistance-capacitance components and the like) can possibly generate problems such as corrosion, softening, deformation, mildew and the like, so that faults such as electric leakage, lightning stroke, short circuit, failure of the components and the like can be caused to the circuit of the circuit board, the quality of the product is affected, the service life is shortened, and potential safety hazards exist to threaten the life safety of people. In order to improve the performance stability and quality reliability of electronic products, it is particularly important to protect the electronic products during the production and manufacturing process.
At present, the circuit board is usually coated with three-proofing paint to protect the circuit board, and the three-proofing paint forms a layer of transparent protective film on the surface of the circuit board, so that circuit faults such as short circuit and the like caused by corrosion and mildew of the circuit board can be avoided, and the quality reliability and the safety coefficient of the circuit board are improved. The three-proofing paint with relatively general market and low price mainly comprises polyurethane, organic silicon, acrylic resin, epoxy resin and other types, but the raw material components of the existing three-proofing paint often contain aromatic solvents such as dimethylbenzene, methylbenzene and the like, have large smell, do not meet VOC emission standards, cause harm to human bodies and have weather resistance to be improved. The aqueous three-proofing paint has the advantages of low price and high performance, but the aqueous polyurethane dispersion is mainly used at present, and the research of the aqueous acrylic three-proofing paint is less. And the defects of the existing water-based acrylic acid are obvious, for example, the mechanical properties of the coating after film formation caused by low solid content can not meet the requirements.
Disclosure of Invention
In order to overcome the defects of the prior art, the purpose of the application is to provide the aqueous acrylic three-proofing paint, wherein the aqueous acrylic resin with specific glass transition temperature (Tg) is adopted as a main raw material, so that the purposes of improving the solid content and the mechanical property of the aqueous three-proofing paint and reducing the cost of the aqueous three-proofing paint are achieved.
In order to solve the problems, the technical scheme adopted by the application is as follows:
the aqueous acrylic three-proofing paint comprises the following components in parts by weight:
70-90 parts of water-based acrylic resin,
6-10 parts of a film forming auxiliary agent,
0.2-0.4 parts of defoaming agent,
0.2 to 0.4 parts of surfactant,
0.2 to 1.0 part of adhesion promoter,
0.05-0.2 parts of fluorescent indicator;
the glass transition temperature of the aqueous acrylic resin is 23-35 ℃.
As a further preferred scheme, the aqueous acrylic resin according to the examples of the present application is prepared from the following components in parts by weight:
15-32 parts of acrylate hard monomer, 12-20 parts of acrylate soft monomer, 5-10 parts of acrylic acid monomer, 2-3 parts of initiator, 10-20 parts of solvent, 5-10 parts of neutralizer and 25-35 parts of water.
As a further preferable scheme, the acrylate hard monomer in the embodiment of the application is one or more of styrene, methyl methacrylate, isobornyl acrylate and isobornyl methacrylate; the acrylic ester soft monomer is one or more than two of butyl acrylate, butyl methacrylate, ethyl acrylate, isooctyl acrylate and isooctyl methacrylate; the acrylic acid monomer is one or a mixture of methacrylic acid and acrylic acid.
As a further preferable scheme, the initiator is one or more than two of azoisobutyronitrile, benzoyl peroxide, diacyl peroxide, tert-butyl peroxide and tert-butyl peroxybenzoate; the solvent is one or a mixture of propylene glycol butyl ether and propylene glycol methyl ether; the neutralizing agent is one or more than two of diethanolamine, ammonia water, triethylamine and dimethylethanolamine.
As a further preferable scheme, the hydroxyl value of the aqueous acrylic resin is controlled to be 10-20 mg KOH/g, the solid content is controlled to be 45% -60%, and the viscosity is controlled to be 200-800 mPa.s.
As a further preferable scheme, the aqueous acrylic resin according to the embodiment of the application is prepared by a three-step method, and the preparation method is as follows
The first step: adding an initiator into a solvent to dissolve, and then dropwise adding the initiator into a mixed solution of an acrylate hard monomer and an acrylate soft monomer to perform polymerization reaction to obtain a first product;
and a second step of: adding a neutralizing agent into the first product to perform a neutralization reaction to obtain a second product;
and a third step of: and dropwise adding deionized water into the second product, and filtering to obtain the water-based acrylic resin with the preset glass transition temperature after high-speed shearing action.
As a further preferred scheme, the reaction procedure in the first step of the embodiment is to carry out solution polymerization at 100-125 ℃, and then raise the temperature to 145-170 ℃ after polymerization to obtain a first product.
As a further preferred embodiment, in the third step described in the examples herein, the high speed shearing is performed at 1200-2000 rpm.
As a further preferable scheme, the film forming auxiliary agent is one or more of benzyl alcohol, ethylene glycol, propylene glycol, hexylene glycol, alcohol ester-12, ethylene glycol butyl ether, propylene glycol methyl ether, propylene glycol ethyl ether, propylene glycol butyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether and tripropylene glycol n-butyl ether; the defoaming agent is one or more than two of BYK-011, BYK-012, BYK-024 and BYK-025; the surfactant is one or two of BYK-345 and BYK-346; the adhesion promoter is one or more than two of aminopropyl trimethoxy silane, aminopropyl triethoxy silane, 3-glycidoxy propyl trimethoxy silane and related silane coupling agent oligomer.
The application also provides a preparation method of the aqueous acrylic three-proofing paint, in the preparation method, the aqueous acrylic resin with proper glass transition temperature is obtained through three-step reaction by selecting acrylic ester raw materials with different glass transition temperatures, and then the aqueous acrylic resin is used as the raw material to prepare the three-proofing paint, so that the problems that the solid content of the existing aqueous three-proofing paint is low and the mechanical property cannot meet the requirement are solved. The preparation method comprises the following steps of,
the three-step method is adopted to prepare the water-based acrylic resin: the first step, an initiator is added into a solvent to be dissolved, and then is added into a mixed solution of an acrylic ester hard monomer and an acrylic ester soft monomer for polymerization reaction, so as to obtain a first product; secondly, adding a neutralizing agent into the first product to perform a neutralization reaction to obtain a second product; thirdly, dropwise adding deionized water into the second product, and filtering to obtain water-based acrylic resin with a preset glass transition temperature after high-speed shearing action;
preparing three-proofing paint: and mixing the aqueous acrylic resin, the film forming auxiliary agent, the defoaming agent, the surfactant, the adhesion promoter and the fluorescent indicator according to the formula amount, and uniformly stirring to obtain the aqueous acrylic three-proofing paint.
Compared with the prior art, the invention has the beneficial effects that:
1. the aqueous acrylic resin with specific glass transition temperature (Tg) adopted by the aqueous acrylic three-proofing paint is used as a main raw material, and the aqueous three-proofing paint is formed after being mixed with a film forming auxiliary agent, a defoaming agent, a surfactant and an adhesion promoter, so that the solid content of the aqueous three-proofing paint is improved, and the purpose of improving the mechanical property of the aqueous three-proofing paint is achieved.
2. The aqueous acrylic three-proofing paint has the advantages of good film forming performance, good dryness, moderate hardness and capability of exerting excellent protective performance in the protection of a circuit board; and because the VOC content is low, the health hazard to constructors is small, and the environment is protected.
3. The aqueous acrylic resin adopted by the application is polymerized by adopting acrylic esters with different glass transition temperatures through a three-step method, and the glass transition temperature of the aqueous acrylic resin can be controlled within a reasonable range through the reaction of the three-step method, so that the requirements of application and performance of the aqueous acrylic resin are met.
4. The preparation method of the water-based acrylic three-proofing paint has simple process and lower cost, so that the price of the product can be reduced, and the industrialized production can be realized, thereby being popularized in market.
The present invention will be described in further detail with reference to the following embodiments.
Detailed Description
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions in the embodiments of the present application will be clearly and completely described below in conjunction with the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present disclosure.
The terms "comprises" and "comprising" and their equivalents, when used in this specification and claims, are intended to cover a non-exclusive inclusion, such that a process or element is not described, but is inherent to the product, method, or structure, but is included in the invention that is expressly described in the specification and claims.
The embodiment of the application provides a water-based acrylic three-proofing paint which comprises the following components in parts by weight:
70-90 parts of water-based acrylic resin,
6-10 parts of a film forming auxiliary agent,
0.2-0.4 parts of defoaming agent,
0.2 to 0.4 parts of surfactant,
0.2 to 1.0 part of adhesion promoter,
0.05-0.2 parts of fluorescent indicator;
the glass transition temperature (Tg) of the aqueous acrylic resin is 23-35 ℃.
[ Water-based acrylic resin ]
In the application, the water-based acrylic resin is used as a raw material of the three-proofing paint, on one hand, the water-based acrylic resin is a low-VOC resin and has high glossiness, weather resistance, chemical resistance and high stability, so that the environment-friendly three-proofing paint can be obtained by using the water-based acrylic resin as the raw material; on the other hand, the aqueous acrylic resin has the defects of high film forming temperature, low film hardness, poor anti-back tack, poor water resistance, poor adhesive force and the like. Therefore, in the examples of the present application, in order to improve the performance of the property three-proofing paint, the glass transition temperature (Tg) of the aqueous acrylic acid used needs to be adjusted. In the specific embodiment of the application, the aqueous acrylic resin adopts acrylic esters with different high and low glass transition temperatures as polymerization monomers, and the aqueous acrylic resin with specific glass transition temperature is synthesized by combining a three-step method by controlling the ratio of the acrylic esters with high glass transition temperature to the acrylic esters with low glass transition temperature, so that the aqueous acrylic resin has the advantages of low VOC, high glossiness, weather resistance, chemical resistance, high stability and the like of the aqueous acrylic resin, and simultaneously improves the solid content and the film forming hardness, reduces the film forming temperature, and simultaneously solves the defects of low hardness, poor back tack resistance, poor water resistance, poor adhesive force and the like of the common aqueous acrylic resin film.
In the present application, the glass transition temperature of the aqueous acrylic resin is an important factor in order to satisfy the properties required for the application. In the process of forming a paint film, the lower the Tg, the better the flexibility of a molecular chain segment, the lower the hardness of the formed paint film, and the poor protective performance; the higher the Tg, the more rigid the molecular chain segment, the better the protective performance of the paint film, but the too large internal stress easily causes the cracking of the paint film. In the application, the glass transition temperature (Tg) of the acrylic resin is regulated to be 23-35 ℃ by regulating the proportioning relation among the components. Preferably, the glass transition temperature (Tg) of the acrylic resin is controlled to 28-35 ℃. Therefore, in the examples of the present application, in order to achieve both flexibility and protective properties, the aqueous acrylic resin used was prepared by a three-step method using the following components in parts by weight:
15-32 parts of acrylate hard monomer, 12-20 parts of acrylate soft monomer, 5-10 parts of acrylic acid monomer, 2-3 parts of initiator, 10-20 parts of solvent, 5-10 parts of neutralizer and 25-35 parts of water.
The first step: and adding the initiator into a solvent to dissolve, and then dropwise adding the initiator into a mixed solution of the acrylate hard monomer and the acrylate soft monomer to perform polymerization reaction to obtain a first product. In some embodiments, the reaction is a solution polymerization at a temperature of 100-125 ℃, followed by a temperature increase of 145-170 ℃ to obtain the first product. Preferably, in some embodiments, the reaction sequence is 115-120 ℃ for solution polymerization.
And a second step of: adding a neutralizing agent into the first product to perform a neutralization reaction to obtain a second product;
and a third step of: and dropwise adding deionized water into the second product, and filtering to obtain the water-based acrylic resin with the preset glass transition temperature after high-speed shearing action. Preferably, in some embodiments, the shearing is performed at a speed of 1200-2000 rpm. It is further preferred that in some embodiments, the shearing is performed at a speed of 1500-1800 rpm.
Further, in some embodiments of the present application, the acrylate hard monomer is selected from, but not limited to, styrene and one or more of methyl methacrylate, isobornyl acrylate, isobornyl methacrylate, and the like; the acrylic ester soft monomer is selected from one or more than two of butyl acrylate, butyl methacrylate, ethyl acrylate, isooctyl methacrylate and the like; the acrylic acid monomer is one or a mixture of methacrylic acid and acrylic acid. In this application, in order to obtain an aqueous acrylic resin with a specific glass transition temperature, in the polymerization reaction, the weight ratio of the hard acrylate monomer to the soft acrylate monomer needs to be controlled, when the weight ratio of the hard acrylate monomer to the soft acrylate monomer is 1: in the range of (0.4-1.35), the glass transition temperature of the obtained aqueous acrylic resin is 30-40 ℃, the hydroxyl value of the aqueous acrylic resin can be controlled to be 10-20 mg KOH/g, the solid content is controlled to be 45-60%, and the viscosity is controlled to be 200-800 mPa.s. Further preferably, the weight ratio of acrylate hard monomer to acrylate soft monomer is 1: (0.8-1.2).
It is further preferable that acrylic acid esters having functional groups such as hydroxyethyl acrylate, hydroxypropyl acrylate, and hydroxybutyl acrylate are further added to the raw material for preparing the aqueous acrylic resin. The addition of the acrylic ester can improve the adhesive force of the water-based acrylic resin and improve the heat resistance and weather resistance of the coating. In some embodiments, the acrylate with functional groups is used in an amount of 1 to 5 parts.
Further, the initiator used in the preparation of the aqueous acrylic resin in the embodiment of the application is selected from one or more than two of azoisobutyronitrile, benzoyl peroxide, diacyl peroxide, tert-butyl peroxybenzoate and the like; the solvent is selected from one or two of propylene glycol butyl ether and propylene glycol methyl ether; the neutralizing agent is selected from one or more than two of diethanolamine, ammonia water, triethylamine and dimethylethanolamine.
[ film Forming auxiliary ]
In the application, the three-proofing paint adopts the water-based acrylic resin as a raw material, and the water-based acrylic resin has better film forming performance, but in the protection of a circuit board, the film forming performance of the three-proofing paint is further improved by adding a film forming auxiliary agent. In this application, alcohols or ethers are used as film forming aids. Preferably, the film forming aid described in the embodiments herein is selected from, but not limited to, benzyl alcohol, ethylene glycol, propylene glycol, hexylene glycol, alcohol ester-12, ethylene glycol butyl ether, propylene glycol methyl ether, propylene glycol ethyl ether, propylene glycol butyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, tripropylene glycol n-butyl ether, or a mixture of two or more thereof.
[ antifoaming agent ]
In the application, the aqueous acrylic three-proofing paint is prepared by adopting an antifoaming agent, and in a specific embodiment, the adopted antifoaming agent is selected from one or more than two of the antifoaming agents of BYK-011, BYK-012, BYK-024, BYK-025 and the like manufactured by Pick chemical company of Germany.
[ surfactant ]
In the application, the water-based acrylic three-proofing paint is prepared by adopting a surfactant, and in a specific embodiment, the surfactant is one or two of BYK-345 and BYK-346 produced by Pick chemical company of Germany.
[ adhesion promoter ]
In the application, the aqueous acrylic tri-proof paint is prepared by adopting an adhesion promoter, preferably, in some embodiments, the adhesion promoter is one or more than two of aminopropyl trimethoxy silane, aminopropyl triethoxy silane, 3-glycidoxy propyl trimethoxy silane and related silane coupling agent oligomer.
The application also provides a preparation method of the aqueous acrylic three-proofing paint, in the preparation method, the aqueous acrylic resin with proper glass transition temperature is obtained through three-step reaction by selecting acrylic ester raw materials with different glass transition temperatures, and then the aqueous acrylic resin is used as the raw material to prepare the three-proofing paint, so that the problems that the solid content of the existing aqueous three-proofing paint is low and the mechanical property cannot meet the requirement are solved. The preparation method comprises the following steps of,
the three-step method is adopted to prepare the water-based acrylic resin: the first step, an initiator is added into a solvent to be dissolved, and then is added into a mixed solution of an acrylic ester hard monomer and an acrylic ester soft monomer for polymerization reaction, so as to obtain a first product; secondly, adding a neutralizing agent into the first product to perform a neutralization reaction to obtain a second product; thirdly, dropwise adding deionized water into the second product, and filtering to obtain water-based acrylic resin with a preset glass transition temperature after high-speed shearing action;
preparing three-proofing paint: and mixing the aqueous acrylic resin, the film forming auxiliary agent, the defoaming agent, the surfactant, the adhesion promoter and the fluorescent indicator according to the formula amount, and uniformly stirring to obtain the aqueous acrylic three-proofing paint.
Specific examples of the present invention are provided below, and the raw materials, equipment, etc. involved in the examples below can be obtained by purchasing them except for special restrictions.
Example 1
The embodiment provides a water-based acrylic three-proofing paint, which is prepared by introducing an acrylic ester soft monomer and an acrylic ester hard monomer into the water-based acrylic three-proofing paint, and comprises the following specific steps: 15g of n-butyl acrylate, 10g of styrene, 17g of methyl methacrylate, 2g of hydroxypropyl acrylate, 6g of methacrylic acid, 2g of azoisobutyronitrile were thoroughly mixed and transferred to a dropping vessel. And (3) adding 15g of propylene glycol diethyl ether into a reaction kettle, stirring and heating to 120 ℃ and refluxing for 20min, dropwise adding the mixed monomer solution, dropwise adding for 3-4 h, preserving heat for 2h after dropwise adding, sampling and testing the conversion rate, cooling to 60 ℃ when the conversion rate is 99%, adding 2.45g of ammonia water neutralizer for neutralization, adding 30g of deionized water, emulsifying for 3h under the shearing action of 1500rpm to obtain the aqueous acrylic resin, and testing relevant performance parameters of the resin. 70 parts of aqueous acrylic resin, 6 parts of film forming auxiliary agent, 0.2 part of defoaming agent, 0.4 part of surfactant, 0.2 part of adhesion promoter and 0.01 part of fluorescent indicator are uniformly mixed to obtain the three-proofing paint.
Example 2
The embodiment provides a water-based acrylic three-proofing paint, which is prepared by introducing an acrylic ester soft monomer and an acrylic ester hard monomer into the water-based acrylic three-proofing paint, and comprises the following specific steps: 20g of n-butyl acrylate, 15g of styrene, 17g of methyl methacrylate, 2g of hydroxypropyl acrylate, 6g of methacrylic acid, 2g of azoisobutyronitrile were thoroughly mixed and transferred to a dropping vessel. And (3) adding 15g of propylene glycol diethyl ether into a reaction kettle, stirring and heating to 120 ℃ and refluxing for 20min, dropwise adding the mixed monomer solution, dropwise adding for 3-4 h, preserving heat for 2h after dropwise adding, sampling and testing the conversion rate, cooling to 60 ℃ when the conversion rate is 99%, adding 2.45g of ammonia water neutralizer for neutralization, adding 30g of deionized water, emulsifying for 3h under the shearing action of 1500rpm to obtain the aqueous acrylic resin, and testing relevant performance parameters of the resin. 85 parts of water-based acrylic resin, 6 parts of film forming auxiliary agent, 0.3 part of defoaming agent, 0.3 part of surfactant, 1.0 part of adhesion promoter and 0.2 part of fluorescent indicator are uniformly mixed to obtain the three-proofing paint.
Example 3
The embodiment provides a water-based acrylic three-proofing paint, which is prepared by introducing an acrylic ester soft monomer and an acrylic ester hard monomer into the water-based acrylic three-proofing paint, and comprises the following specific steps: 15g of n-butyl acrylate, 20g of styrene, 17g of methyl methacrylate, 2g of hydroxypropyl acrylate, 6g of methacrylic acid, 2g of azoisobutyronitrile were thoroughly mixed and transferred to a dropping vessel. And (3) adding 15g of propylene glycol diethyl ether into a reaction kettle, stirring and heating to 120 ℃ and refluxing for 20min, dropwise adding the mixed monomer solution, dropwise adding for 3-4 h, preserving heat for 2h after dropwise adding, sampling and testing the conversion rate, cooling to 60 ℃ when the conversion rate is 99%, adding 2.45g of ammonia water neutralizer for neutralization, adding 30g of deionized water, emulsifying for 3h under the shearing action of 1500rpm to obtain the aqueous acrylic resin, and testing relevant performance parameters of the resin. 90 parts of aqueous acrylic resin, 8 parts of film forming auxiliary agent, 0.4 part of defoaming agent, 0.4 part of surfactant, 0.5 part of adhesion promoter and 0.2 part of fluorescent indicator are uniformly mixed to obtain the three-proofing paint.
Example 4
The embodiment provides a water-based acrylic three-proofing paint, which is prepared by introducing an acrylic ester soft monomer and an acrylic ester hard monomer into the water-based acrylic three-proofing paint, and comprises the following specific steps: 15g of n-butyl acrylate, 15g of styrene, 22g of methyl methacrylate, 2g of hydroxypropyl acrylate, 6g of methacrylic acid, 2g of azoisobutyronitrile were thoroughly mixed and transferred to a dropping vessel. 15g of propylene glycol diethyl ether is put into a reaction kettle, stirred and heated to 120 ℃ and refluxed for 20min, the mixed monomer solution is dropwise added, 3-4 h is dropwise added, the temperature is kept for 2h after the dropwise addition, the sample is taken to test the conversion rate, when the conversion rate is 99%, the sample is cooled to 60 ℃, 2.45g of ammonia water neutralizer is added for neutralization, 30g of deionized water is added for emulsification for 3h under the shearing action of 1500rpm, the aqueous acrylic resin is obtained, and the relevant performance parameters of the resin are tested, and the aqueous acrylic resin, the film forming auxiliary agent, the defoaming agent, the surfactant, the adhesion promoter and the fluorescent indicator are uniformly mixed according to the proportion of the embodiment 2, so that the three-proofing paint is obtained.
Comparative example 1
For comparison with the protocol of the present application, in this comparative example, the aqueous acrylic resin was prepared without introducing acrylate hard monomers. The specific method comprises the following steps: 30g of n-butyl acrylate, 22g of ethylhexyl acrylate, 6g of methacrylic acid, 2g of hydroxypropyl acrylate, 2g of azoisobutyronitrile were thoroughly mixed and transferred to a dropping vessel. And (3) adding 15g of propylene glycol diethyl ether into a reaction kettle, stirring and heating to 120 ℃ and refluxing for 20min, dropwise adding the mixed monomer solution, dropwise adding for 3-4 h, preserving heat for 2h after dropwise adding, sampling and testing the conversion rate, cooling to 60 ℃ when the conversion rate is 99%, adding 2.45g of ammonia water neutralizer for neutralization, adding 30g of deionized water, emulsifying for 3h under the shearing action of 1500rpm to obtain the aqueous acrylic resin, and testing relevant performance parameters of the resin. The aqueous acrylic resin, the film-forming auxiliary agent, the defoamer, the surfactant, the adhesion promoter and the fluorescent indicator are uniformly mixed according to the proportion of the embodiment 2 to obtain the three-proofing paint.
Comparative example 2
For comparison with the protocol of the present application, in this comparative example, the aqueous acrylic resin was prepared without introducing the acrylate soft monomer. 35g of styrene, 17g of methyl methacrylate, 6g of methacrylic acid, 2g of hydroxypropyl acrylate, 2g of azoisobutyronitrile were thoroughly mixed and transferred to a dropping vessel. And (3) adding 15g of propylene glycol diethyl ether into a reaction kettle, stirring and heating to 120 ℃ and refluxing for 20min, dropwise adding the mixed monomer solution, dropwise adding for 3-4 h, preserving heat for 2h after dropwise adding, sampling and testing the conversion rate, cooling to 60 ℃ when the conversion rate is 99%, adding 2.45g of ammonia water neutralizer for neutralization, adding 30g of deionized water, emulsifying for 3h under the shearing action of 1500rpm to obtain the aqueous acrylic resin, and testing relevant performance parameters of the resin. The aqueous acrylic resin, the film-forming auxiliary agent, the defoamer, the surfactant, the adhesion promoter and the fluorescent indicator are uniformly mixed according to the proportion of the embodiment 2 to obtain the three-proofing paint.
Performance testing
1. The aqueous acrylic resins obtained in examples 1 to 4 and comparative examples 1 to 2 were subjected to performance test, and the results are shown in Table 1.
Table 1: results of the Water-based acrylic resin Performance parameter test
Examples Example 1 Example 2 Example 3 Example 4 Comparative example 1 Comparative example 2
Viscosity (mPas) 400 460 620 545 350 800
Solid content (%) 50 50 56 53 47 50
Hydroxyl value (mgKOH/g) 14 16 15 15 15 15
T g （℃） 15 23 35 28 2 60
2. The properties of the three-proofing paints obtained in examples 1 to 4 and comparative examples 1 to 2 were tested by coating the three-proofing paint on a test board and testing the three-proofing paint properties according to the IPC-CC-830C standard after curing for 7 d. The test results are shown in Table 2.
Table 2: performance test result of three-proofing paint
Examples Example 1 Example 2 Example 3 Example 4 Comparative example 1 Comparative example 2
Appearance @ visual Milk white Milk white Milk white Milk white Milk white Milk white
Viscosity (mPas) 220 250 300 320 200 150
Fluorescence (365 nm) Blue light Blue light Blue light Blue light Blue light Blue light
Film Forming Property @25 DEG C Good (good) Good (good) Good (good) Good (good) Good (good) Poor quality
Surface drying time (min) @25 DEG C 10 15 30 25 5 60
Hardness (Pencil hardness) 3B 2B HB B 5B 2H
Adhesion force Level 0 Level 0 Level 0 Level 0 Level 0 3 grade
Mildew resistance (28 d type strain) Not pass through By passing through By passing through By passing through Not pass through By passing through
Insulation volume resistance (omega cm) 10 13 10 13 10 13 10 13 10 13 10 13
Flexibility (1 mm) By passing through By passing through By passing through By passing through By passing through Not pass through
UL 94 flame retardance HB HB HB HB HB HB
Dielectric strength (kV/mm) 14 16 20 18 12 28
Cold and hot impact (300 h) By passing through By passing through By passing through By passing through By passing through Not pass through
Neutral salt fog time (384 h) By passing through By passing through By passing through By passing through Not pass through Not pass through
Damp-heat resistant time (384 h) By passing through By passing through By passing through By passing through Not pass through Not pass through
As is evident from the above test results, T of the aqueous acrylic resin g The value design is the key to influence the performance of the water-based three-proofing paint. T (T) g Too low, although film forming property is good, surface drying time is fast, hardness of a paint film is low, flexibility is good, and most of protective performance is greatly reduced. The higher the Tg value, the higher the surface hardness, but too poor adhesion can also affect the performance of the aqueous three-proofing paint. From the comprehensive embodiment, when the Tg value of the water-based acrylic resin is set at 23-35 ℃, the film forming property, the surface drying time, the mechanical property and the protective property are all better. In the experimental process, the embodiment 3 is the best preferable scheme in the invention, the duration of cold and hot impact, neutral salt fog resistance and wet heat resistance in the embodiment 3 is 2-3 times of the IPC-CC-830C standard, the performance of the paint is equivalent to that of solvent-based three-proofing paint, and the paint is hopeful to replace solvent-based three-proofing paint with high VOC content.
The embodiments described above are merely preferred embodiments of the present invention, and are not intended to limit the scope of the present invention, so that any insubstantial changes and substitutions made by those skilled in the art on the basis of the present invention are within the scope of the claimed invention.

Claims (10)

1. The aqueous acrylic three-proofing paint is characterized by comprising the following components in parts by weight:
70-90 parts of water-based acrylic resin,
6-10 parts of a film forming auxiliary agent,
0.2-0.4 parts of defoaming agent,
0.2 to 0.4 parts of surfactant,
0.2 to 1.0 part of adhesion promoter,
0.05-0.2 parts of fluorescent indicator;
the glass transition temperature of the aqueous acrylic resin is 23-35 ℃.
2. The aqueous acrylic three-proofing paint according to claim 1, wherein the aqueous acrylic resin is prepared from the following components in parts by weight:
15-32 parts of acrylate hard monomer, 12-20 parts of acrylate soft monomer, 5-10 parts of acrylic acid monomer, 2-3 parts of initiator, 10-20 parts of solvent, 5-10 parts of neutralizer and 25-35 parts of water.
3. The aqueous acrylic three-proofing paint according to claim 2, wherein the acrylate hard monomer is one or more of styrene, methyl methacrylate, isobornyl acrylate and isobornyl methacrylate; the acrylic ester soft monomer is one or more than two of butyl acrylate, butyl methacrylate, ethyl acrylate, isooctyl acrylate and isooctyl methacrylate; the acrylic acid monomer is one or a mixture of methacrylic acid and acrylic acid.
4. The aqueous acrylic tri-proof paint of claim 2, wherein the initiator is one or more of azoisobutyronitrile, benzoyl peroxide, diacyl peroxide, t-butyl peroxybenzoate; the solvent is one or a mixture of propylene glycol butyl ether and propylene glycol methyl ether; the neutralizing agent is one or more than two of diethanolamine, ammonia water, triethylamine and dimethylethanolamine.
5. The aqueous acrylic three-proofing paint according to claim 2, wherein the hydroxyl value of the aqueous acrylic resin is controlled to be 10-20 mg KOH/g, the solid content is controlled to be 45-60%, and the viscosity is controlled to be 200-800 mPa.s.
6. The aqueous acrylic three-proofing paint according to claim 2, wherein the aqueous acrylic resin is prepared by a three-step method, and the preparation method comprises the following steps of
The first step: adding an initiator into a solvent to dissolve, and then dropwise adding the initiator into a mixed solution of an acrylate hard monomer and an acrylate soft monomer to perform polymerization reaction to obtain a first product;
and a second step of: adding a neutralizing agent into the first product to perform a neutralization reaction to obtain a second product;
and a third step of: and dropwise adding deionized water into the second product, and filtering to obtain the water-based acrylic resin with the preset glass transition temperature after high-speed shearing action.
7. The aqueous acrylic three-proofing paint according to claim 6, wherein the reaction procedure in the first step is solution polymerization at 100-125 ℃, and the temperature is raised to 145-170 ℃ after the polymerization to obtain the first product.
8. The aqueous acrylic tri-proof paint of claim 6, wherein in the third step, the high speed shearing is performed at 1200-2000 rpm.
9. The aqueous acrylic tri-proof paint of any one of claims 1 to 5, wherein the film forming aid is one or more of benzyl alcohol, ethylene glycol, propylene glycol, hexylene glycol, alcohol ester-12, ethylene glycol butyl ether, propylene glycol methyl ether, propylene glycol ethyl ether, propylene glycol butyl ether, dipropylene glycol monomethyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, tripropylene glycol n-butyl ether; the defoaming agent is one or more than two of BYK-011, BYK-012, BYK-024 and BYK-025; the surfactant is one or two of BYK-345 and BYK-346; the adhesion promoter is one or more than two of aminopropyl trimethoxy silane, aminopropyl triethoxy silane, 3-glycidoxy propyl trimethoxy silane and related silane coupling agent oligomer.
10. A method for preparing the aqueous acrylic tri-proof paint as claimed in any one of claims 1 to 9, comprising
The three-step method is adopted to prepare the water-based acrylic resin: the first step, an initiator is added into a solvent to be dissolved, and then is added into a mixed solution of an acrylic ester hard monomer and an acrylic ester soft monomer for polymerization reaction, so as to obtain a first product; secondly, adding a neutralizing agent into the first product to perform a neutralization reaction to obtain a second product; thirdly, dropwise adding deionized water into the second product, and filtering to obtain water-based acrylic resin with a preset glass transition temperature after high-speed shearing action;
preparing three-proofing paint: and mixing the aqueous acrylic resin, the film forming auxiliary agent, the defoaming agent, the surfactant, the adhesion promoter and the fluorescent indicator according to the formula amount, and uniformly stirring to obtain the aqueous acrylic three-proofing paint.
CN202310704635.9A 2023-06-14 2023-06-14 Water-based acrylic three-proofing paint and preparation method thereof Pending CN116426186A (en)

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