CN111944377A - Multifunctional water-based epoxy acrylic resin composition and preparation method thereof - Google Patents
Multifunctional water-based epoxy acrylic resin composition and preparation method thereof Download PDFInfo
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- CN111944377A CN111944377A CN202010857953.5A CN202010857953A CN111944377A CN 111944377 A CN111944377 A CN 111944377A CN 202010857953 A CN202010857953 A CN 202010857953A CN 111944377 A CN111944377 A CN 111944377A
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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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/003—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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- 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
- C08F265/00—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00
- C08F265/02—Macromolecular compounds obtained by polymerising monomers on to polymers of unsaturated monocarboxylic acids or derivatives thereof as defined in group C08F20/00 on to polymers of acids, salts or anhydrides
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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
- 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
Abstract
A multifunctional water-based epoxy acrylic resin composition and a preparation method thereof are obtained by copolymerizing modified bisphenol A epoxy resin and a core-shell structure acrylic prepolymer, and are prepared by the following steps: (1) mixing bisphenol A type epoxy resin with monoacid or diacid to obtain modified bisphenol A type epoxy resin; (2) sequentially adding acrylic acid, styrene, acrylonitrile and water into a reaction kettle to obtain emulsion A; (3) adding acrylic acid, styrene, acrylonitrile and a molecular weight regulator into the emulsion A to react to obtain a core-shell structure acrylic prepolymer; (4) mixing the acrylic prepolymer and the modified bisphenol A epoxy resin for reaction to obtain a multifunctional aqueous epoxy acrylic resin composition; the acrylic resin is modified by the epoxy resin, and the excessive crosslinking of the epoxy resin and the acrylic resin is prevented by adopting a two-step reaction, so that the resin composition has high water solubility, excellent adhesive force, high hydrolysis resistance, high film forming strength and excellent wear resistance, acid resistance and alkali resistance.
Description
Technical Field
The invention belongs to the technical field of coatings, and particularly relates to a multifunctional water-based epoxy acrylic resin composition and a preparation method thereof.
Background
The coating used by metal materials or inorganic non-metal materials and the like occupies the largest share in the coating market, the original solvent-based coating always takes organic solvents such as toluene, xylene, trimethylbenzene, ethyl acetate, butyl acetate, cyclohexanone and the like as diluents, the smell is large, the coating is harmful to the health of people, the environmental pollution and the like, and the emission of pollutants is strictly controlled by environmental protection departments. From the production manufacturing, application of painting, once the management is neglected, the combustion explosion is easy to be caused, and the method belongs to the dangerous chemical supervision product. The water-soluble coating avoids the risks, greatly reduces the discharge of VOC, greatly saves petroleum resources by replacing solvent with water, is a novel environment-friendly product, and also belongs to non-dangerous chemicals.
At present, solvent-type acrylic resin products play an important role in China, but the solvent-type acrylic resin is not friendly to the environment and human health due to high VOC value, so that the solvent-type acrylic resin is in danger of exiting the market. Therefore, aqueous acrylic resins are preferred; the water-based acrylic resin has the advantages of no pollution, no toxicity, no irritation, better gloss, good chemical resistance, high stability, safe production, low price and the like, but has the defect of indelibility, and is mainly characterized by hot adhesion, cold brittleness, poor anti-tack property, poor heat resistance, short water resistance, poor impact resistance and the like after the film of the resin is formed and dried, so that the application field of the water-based acrylic resin is limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a multifunctional water-based epoxy acrylic resin composition which is obtained by copolymerizing modified bisphenol A epoxy resin and a core-shell structure acrylic prepolymer.
A preparation method of a multifunctional water-based epoxy acrylic resin composition comprises the following steps:
the method comprises the following steps: mixing bisphenol A epoxy resin with a molar ratio of 1: 0.5-1.0 with monoacid or diacid, taking a mixture of propylene glycol ether and cyclohexanone with a mass ratio of 1:1 as a solvent, adding a catalyst, heating the material to 150 ℃ and 170 ℃ in a reflux state, preserving heat for 2-4h, and stopping heating when the acid value is reduced to below 1mgKOH/g to obtain modified bisphenol A epoxy resin;
step two: sequentially adding 3-8 parts of acrylic acid, 2-7 parts of styrene, 4-6 parts of acrylonitrile and 38-65 parts of water into a reaction kettle, and adding an emulsifier for emulsification for 20-30 min; adding 1-2 parts of initiator into water for dissolving, dropwise adding 30% of initiator solution into a reaction kettle for 1-2h, heating the materials to 70-80 ℃, and stirring for reacting for 0.5-1.5h to obtain emulsion A;
step three: respectively adding 6-12 parts of acrylic acid, 2-6 parts of styrene, 1.5-7.5 parts of acrylonitrile and 0.3-0.5 part of molecular weight regulator into the emulsion A, dropwise adding the rest 70% of initiator solution into a reaction kettle for 1-2h, simultaneously heating the materials to 75-85 ℃, and stirring for reaction for 2-3h to obtain the acrylic prepolymer with the core-shell structure;
step four: mixing the core-shell structure acrylic prepolymer with the modified bisphenol A epoxy resin in a molar ratio of 1 (0.4-0.75), adding a catalyst and a crosslinking agent after uniform mixing, reacting for 1.5-3h at 90-120 ℃, neutralizing by using a neutralizing agent, and diluting by using deionized water to obtain the multifunctional aqueous epoxy acrylic resin composition.
Preferably, the catalyst is triphenylphosphine or amine catalyst, and the using amount of the catalyst is 0.5-1.5% of the mass of the diacid A type epoxy resin.
Preferably, the bisphenol A type epoxy resin is at least one of E-12, E-14 and E-20.
Preferably, the mono-or dibasic acid is at least one of n-hexanoic acid, n-octanoic acid, benzoic acid, phthalic acid, isophthalic acid, sebacic acid, and adipic acid.
Preferably, the emulsifier is any one of sulfosuccinic acid and octyl phenol polyoxyethylene ether.
Preferably, the molecular weight regulator is n-dodecyl mercaptan.
Preferably, the neutralizing agent is at least one of triethylamine, dimethylethanolamine and 2-amino-2-methyl-1-propanol.
Has the advantages that:
according to the multifunctional water-based epoxy acrylic resin composition, the modified bisphenol A epoxy resin is compounded with the core-shell structure acrylic prepolymer, and the core-shell structure acrylic prepolymer at least has two-layer structures of a hydrophobic core and a hydrophilic surface coating, so that the prepared water-based acrylic resin has good hydrophilicity and good water resistance; the epoxy resin for the acrylic resin is modified, and a two-step reaction is adopted, so that excessive crosslinking of the epoxy resin and the acrylic resin in the modification process is prevented, the molecular weight balance of a product and the structure of the resin are ensured, the active groups on each molecular chain of the product are ensured to be distributed in a balanced manner, the water-based degree of the product is easy, the storage stability of the product is improved, the resin composition has high water solubility, excellent adhesive force, high hydrolysis resistance, high film forming strength and excellent wear resistance and acid and alkali resistance, and the water-based resin enables the water-based paint to replace and adapt to the application environment of the oil paint while reducing environmental pollution, and the excellent performance of the water-based paint is exerted.
Detailed Description
For the purpose of enhancing understanding of the present invention, the present invention will be further described in detail with reference to the following examples, which are provided for illustration only and are not to be construed as limiting the scope of the present invention.
The multifunctional water-based epoxy acrylic resin composition is characterized by being obtained by copolymerizing modified bisphenol A epoxy resin and a core-shell structure acrylic prepolymer.
Example 1
A preparation method of a multifunctional water-based epoxy acrylic resin composition comprises the following steps:
the method comprises the following steps: mixing bisphenol A epoxy resin with a molar ratio of 1:0.8 and monoacid or diacid, taking a mixture of propylene glycol ether and cyclohexanone with a mass ratio of 1:1 as a solvent, adding a catalyst, heating the material to 160 ℃ in a reflux state, preserving the temperature for 2.5 hours, and stopping heating when the acid value is reduced to below 1mgKOH/g to obtain modified bisphenol A epoxy resin;
step two: adding 7 parts of acrylic acid, 5 parts of styrene, 4 parts of acrylonitrile and 45 parts of water into a reaction kettle in sequence, and adding an emulsifier for emulsification for 28 min; adding 1.5 parts of initiator into water for dissolving, dropwise adding 30% of initiator solution into a reaction kettle by mass for 1.5h, heating the materials to 75 ℃, and stirring for reacting for 1.5h to obtain emulsion A;
step three: respectively adding 10 parts of acrylic acid, 6 parts of styrene, 7 parts of acrylonitrile and 0.5 part of molecular weight regulator into the emulsion A, dropwise adding the rest 70% of initiator solution into a reaction kettle for 1.5h, heating the materials to 80 ℃, and stirring for reaction for 3h to obtain the core-shell structure acrylic prepolymer;
step four: mixing the core-shell structure acrylic prepolymer and the modified bisphenol A epoxy resin in a molar ratio of 1:0.65, adding a catalyst and a crosslinking agent after uniform mixing, reacting for 2 hours at 120 ℃, neutralizing by using a neutralizing agent, and diluting by using deionized water to obtain the multifunctional water-based epoxy acrylic resin composition.
Example 2
A preparation method of a multifunctional water-based epoxy acrylic resin composition comprises the following steps:
the method comprises the following steps: mixing bisphenol A epoxy resin with a molar ratio of 1:1.0 and monoacid or diacid, taking a mixture of propylene glycol ether and cyclohexanone with a mass ratio of 1:1 as a solvent, adding a catalyst, heating the material to 155 ℃ in a reflux state, preserving heat for 3 hours, and stopping heating when the acid value is reduced to below 1mgKOH/g to obtain modified bisphenol A epoxy resin;
step two: sequentially adding 8 parts of acrylic acid, 6 parts of styrene, 5 parts of acrylonitrile and 55 parts of water into a reaction kettle, and adding an emulsifier for emulsification for 25 min; adding 2 parts of initiator into water for dissolving, dropwise adding 30% of initiator solution into a reaction kettle by mass for 1h, heating the materials to 80 ℃, and stirring for reacting for 1.2h to obtain emulsion A;
step three: respectively adding 9 parts of acrylic acid, 3 parts of styrene, 6.5 parts of acrylonitrile and 0.3 part of molecular weight regulator into the emulsion A, dropwise adding the rest 70% of initiator solution into a reaction kettle for 2 hours, heating the materials to 75 ℃, and stirring for reaction for 2.5 hours to obtain the acrylic prepolymer with the core-shell structure;
step four: mixing the core-shell structure acrylic prepolymer and the modified bisphenol A epoxy resin in a molar ratio of 1:0.7, adding a catalyst and a crosslinking agent after uniform mixing, reacting for 2.5 hours at 95 ℃, neutralizing by a neutralizing agent, and diluting by deionized water to obtain the multifunctional water-based epoxy acrylic resin composition.
Example 3
A preparation method of a multifunctional water-based epoxy acrylic resin composition comprises the following steps:
the method comprises the following steps: mixing bisphenol A epoxy resin with a molar ratio of 1:1.0 and monoacid or diacid, taking a mixture of propylene glycol ether and cyclohexanone with a mass ratio of 1:1 as a solvent, adding a catalyst, heating the material to 170 ℃ in a reflux state, preserving heat for 3.5 hours, and stopping heating when the acid value is reduced to below 1mgKOH/g to obtain modified bisphenol A epoxy resin;
step two: sequentially adding 6 parts of acrylic acid, 4 parts of styrene, 4 parts of acrylonitrile and 60 parts of water into a reaction kettle, and adding an emulsifier for emulsification for 26 min; adding 1.5 parts of initiator into water for dissolving, dropwise adding 30% of initiator solution into a reaction kettle by mass for 1.5h, simultaneously heating the materials to 80 ℃, and stirring for reacting for 1.0h to obtain emulsion A;
step three: respectively adding 12 parts of acrylic acid, 5 parts of styrene, 7.5 parts of acrylonitrile and 0.5 part of molecular weight regulator into the emulsion A, dropwise adding the rest 70% of initiator solution into a reaction kettle for 1.5h, heating the materials to 80 ℃, and stirring for reaction for 2.5h to obtain the acrylic prepolymer with the core-shell structure;
step four: mixing the core-shell structure acrylic prepolymer and the modified bisphenol A epoxy resin in a molar ratio of 1:0.65, adding a catalyst and a crosslinking agent after uniform mixing, reacting for 2.5 hours at 100 ℃, neutralizing by a neutralizing agent, and diluting by deionized water to obtain the multifunctional water-based epoxy acrylic resin composition.
Example 4
This example is intended to demonstrate the performance of waterborne corrosion resistant coatings prepared from the waterborne epoxy ester resin compositions obtained in examples 1-3, and the waterborne corrosion resistant coatings were prepared as follows:
(1) adding 250g of water into a reaction kettle, then adding 3.5g of water-based dispersing agent, 3.1g of foam inhibitor, 2.8g of anti-settling agent, 2.7g of flatting agent and 1.5g of adhesion promoter into the reaction kettle, and stirring for 15-20min at 600-800 rpm;
(2) adding 200g of the waterborne epoxy acrylic resin composition into a reaction kettle, then sequentially adding 3.0g of zinc phosphate, 1.5g of cosolvent and 1.9g of defoamer, stirring at 800rpm for 20-30min at 600-.
Directly coating the sample prepared in the embodiment 1-3 on the surface of a metal plate, and naturally drying the surface; the corrosion resistance of the obtained water-based anticorrosive coating is shown in the following table:
table 1: water-based anticorrosive paint performance prepared from water-based epoxy acrylic resin composition
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (8)
1. The multifunctional water-based epoxy acrylic resin composition is characterized by being obtained by copolymerizing modified bisphenol A epoxy resin and a core-shell structure acrylic prepolymer.
2. The preparation method of the multifunctional waterborne epoxy acrylic resin composition as claimed in claim 1, which is characterized by comprising the following steps:
the method comprises the following steps: mixing bisphenol A epoxy resin with a molar ratio of 1: 0.5-1.0 with monoacid or diacid, taking a mixture of propylene glycol ether and cyclohexanone with a mass ratio of 1:1 as a solvent, adding a catalyst, heating the material to 150 ℃ and 170 ℃ in a reflux state, preserving heat for 2-4h, and stopping heating when the acid value is reduced to below 1mgKOH/g to obtain modified bisphenol A epoxy resin;
step two: sequentially adding 3-8 parts of acrylic acid, 2-7 parts of styrene, 4-6 parts of acrylonitrile and 38-65 parts of water into a reaction kettle, and adding an emulsifier for emulsification for 20-30 min; adding 1-2 parts of initiator into water for dissolving, dropwise adding 30% of initiator solution into a reaction kettle for 1-2h, heating the materials to 70-80 ℃, and stirring for reacting for 0.5-1.5h to obtain emulsion A;
step three: respectively adding 6-12 parts of acrylic acid, 2-6 parts of styrene, 1.5-7.5 parts of acrylonitrile and 0.3-0.5 part of molecular weight regulator into the emulsion A, dropwise adding the rest 70% of initiator solution into a reaction kettle for 1-2h, simultaneously heating the materials to 75-85 ℃, and stirring for reaction for 2-3h to obtain the acrylic prepolymer with the core-shell structure;
step four: mixing the core-shell structure acrylic prepolymer with the modified bisphenol A epoxy resin in a molar ratio of 1 (0.4-0.75), adding a catalyst and a crosslinking agent after uniform mixing, reacting for 1.5-3h at 90-120 ℃, neutralizing by using a neutralizing agent, and diluting by using deionized water to obtain the multifunctional aqueous epoxy acrylic resin composition.
3. The multifunctional aqueous epoxy acrylic resin composition as claimed in claim 2, wherein the catalyst is triphenylphosphine or an amine catalyst, and the amount of the catalyst is 0.5-1.5% of the weight of the diacid A epoxy resin.
4. The multifunctional aqueous epoxy acrylic resin composition according to claim 2, wherein the bisphenol a type epoxy resin is at least one of E-12, E-14, and E-20.
5. The multifunctional aqueous epoxy acrylic resin composition according to claim 2, wherein the mono-or dibasic acid is at least one of n-hexanoic acid, n-octanoic acid, benzoic acid, phthalic acid, isophthalic acid, sebacic acid, and adipic acid.
6. The multifunctional aqueous epoxy acrylic resin composition according to claim 2, wherein the emulsifier is any one of sulfosuccinic acid and octylphenol polyoxyethylene ether.
7. The multifunctional aqueous epoxy acrylic resin composition according to claim 2, wherein the molecular weight regulator is n-dodecyl mercaptan.
8. The multifunctional aqueous epoxy acrylic resin composition according to claim 2, wherein the neutralizing agent is at least one of triethylamine, dimethylethanolamine, 2-amino-2-methyl-1-propanol.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113831541A (en) * | 2021-09-23 | 2021-12-24 | 无锡拜纳高分子材料科技有限公司 | Preparation process of nano core-shell particle toughening modified epoxy resin |
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| CN101851396A (en) * | 2009-06-12 | 2010-10-06 | 北京金汇利应用化工制品有限公司 | Waterborne epoxy ester resin composition and preparation method thereof and water-based paint prepared from same |
| CN102399350A (en) * | 2011-09-16 | 2012-04-04 | 北京红狮漆业有限公司 | Aqueous epoxy acrylate resin and preparation method thereof |
| CN105085769A (en) * | 2015-02-13 | 2015-11-25 | 陶栋梁 | Aqueous acrylic resin and preparation method thereof |
| CN106084241A (en) * | 2016-05-30 | 2016-11-09 | 山东齐鲁漆业有限公司 | A kind of preparation method and applications of aqueous acrylic modified epoxy ester resin |
| CN107163179A (en) * | 2017-04-11 | 2017-09-15 | 河北晨阳工贸集团有限公司 | Hud typed environment-friendly water-based high finish coat varnish of acrylic emulsion and zero VOC and preparation method thereof |
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2020
- 2020-08-24 CN CN202010857953.5A patent/CN111944377A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4212776A (en) * | 1978-10-16 | 1980-07-15 | Mobil Oil Corporation | Self crosslinking water dispersible epoxy ester-acrylate polymers |
| CN101851396A (en) * | 2009-06-12 | 2010-10-06 | 北京金汇利应用化工制品有限公司 | Waterborne epoxy ester resin composition and preparation method thereof and water-based paint prepared from same |
| CN102399350A (en) * | 2011-09-16 | 2012-04-04 | 北京红狮漆业有限公司 | Aqueous epoxy acrylate resin and preparation method thereof |
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| CN107163179A (en) * | 2017-04-11 | 2017-09-15 | 河北晨阳工贸集团有限公司 | Hud typed environment-friendly water-based high finish coat varnish of acrylic emulsion and zero VOC and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113831541A (en) * | 2021-09-23 | 2021-12-24 | 无锡拜纳高分子材料科技有限公司 | Preparation process of nano core-shell particle toughening modified epoxy resin |
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