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CN108165128B - Double-component water-based epoxy coating and preparation method and application thereof - Google Patents

Double-component water-based epoxy coating and preparation method and application thereof Download PDF

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CN108165128B
CN108165128B CN201711238329.1A CN201711238329A CN108165128B CN 108165128 B CN108165128 B CN 108165128B CN 201711238329 A CN201711238329 A CN 201711238329A CN 108165128 B CN108165128 B CN 108165128B
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based epoxy
stirring
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CN108165128A (en
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张胜
王振兴
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Guangzhou Leobo Paint Science & Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D163/00Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14Polycondensates modified by chemical after-treatment
    • C08G59/1433Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
    • C08G59/1438Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14Polycondensates modified by chemical after-treatment
    • C08G59/1433Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
    • C08G59/1438Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing oxygen
    • C08G59/1455Monocarboxylic acids, anhydrides, halides, or low-molecular-weight esters thereof
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14Polycondensates modified by chemical after-treatment
    • C08G59/1433Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds
    • C08G59/1477Polycondensates modified by chemical after-treatment with organic low-molecular-weight compounds containing nitrogen
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/14Polycondensates modified by chemical after-treatment
    • C08G59/1494Polycondensates modified by chemical after-treatment followed by a further chemical treatment thereof
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16Antifouling paints; Underwater paints
    • C09D5/1656Antifouling paints; Underwater paints characterised by the film-forming substance
    • C09D5/1662Synthetic film-forming substance
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16Antifouling paints; Underwater paints
    • C09D5/1687Use of special additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • C08K2003/2241Titanium dioxide

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  • Polymers & Plastics (AREA)
  • Wood Science & Technology (AREA)
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Abstract

The invention discloses a two-component water-based epoxy coating and a preparation method and application thereof, wherein the two-component water-based epoxy coating comprises the following components in parts by mass: the component A comprises: 20-36 parts by mass of deionized water; 11-4 parts by mass of an auxiliary agent; 22-50 parts of pigment and filler; 25-40 parts by mass of a water-based epoxy curing agent; the component B comprises: 10-40 parts by mass of deionized water; 20.8-2 parts by mass of an auxiliary agent; 50-90 parts by mass of self-made waterborne epoxy resin. The double-component coating can meet the requirement of interior decoration, can be used as water-based epoxy wall paint, has good stain resistance effect and strong isolation, and can meet the requirement of high-cleanness decoration.

Description

Double-component water-based epoxy coating and preparation method and application thereof
Technical Field
The invention relates to the field of building coatings, in particular to a two-component coating and a preparation method and application thereof.
Technical Field
In 2016, the demand of the coating in China is as high as 1800 million tons, wherein the using amount of the water paint only accounts for 10 percent, while the proportion of the water paint in Europe and America is as high as 80 percent, the water paint market space is unlimited as the first major world coating in China, and the water-based property of the coating is a great trend of the current coating world. Epoxy resin is widely applied in the coating industry, but most of the epoxy resin is solvent type, a large amount of organic solvents such as ketones, aromatic hydrocarbons and the like are needed to be used as diluents, the odor is large, the volatilization is easy, and the pollution to the surrounding environment is great. Along with the increasing importance of people on the environment and the increasing requirements on the environmental protection, the research on the water-based epoxy resin is more and more important, and the coating using the water-based epoxy resin as a main film forming substance is water-based, environment-friendly and has strong functionality. However, the existing water-based epoxy coating on the market also has the defects of poor stability, water resistance, scrubbing resistance, stain resistance and the like.
Disclosure of Invention
Based on the above, the present invention aims to overcome the defects of the prior art and provide a two-component water-based epoxy coating which has excellent scrub resistance, stain resistance and isolation.
The invention also aims to provide a preparation method of the two-component water-based epoxy coating.
The invention also aims to provide application of the two-component water-based epoxy coating.
The technical scheme is as follows:
a two-component water-based epoxy coating comprises the following components in parts by mass:
the component A comprises:
Figure BDA0001489429690000011
the component B comprises:
10-40 parts by mass of deionized water;
20.8-2 parts by mass of an auxiliary agent;
50-90 parts by mass of self-made waterborne epoxy resin;
the preparation method of the self-made waterborne epoxy resin comprises the following steps:
s1, reacting epoxy resin E-44 with diisocyanate to obtain modified epoxy resin with terminal group containing isocyanate group;
s2, reacting the modified epoxy resin with the terminal group containing isocyanic acid radical with polycaprolactone and micromolecule dihydric alcohol to obtain polyurethane modified epoxy resin;
s3, reacting with dimethylolbutyric acid to introduce carboxyl into the polyurethane modified epoxy resin;
s4, end capping with epoxy resin E-51, oxidizing with hydrogen peroxide, and adding a solvent to reduce viscosity;
and S5, adding caustic soda for neutralization, adding a nonionic emulsifier to emulsify the system, vacuumizing to remove the solvent in the system, and standing to obtain the anionic waterborne epoxy resin emulsion.
According to the invention, hydrophilic groups are introduced into a molecular chain by a prepolymer method, the prepolymer with epoxy groups at both ends of the molecular chain and at the end functional groups of the side chain is synthesized, salt is synthesized in caustic soda, and the hydrophilic groups extend to a water phase to wrap the epoxy groups in emulsion colloidal particles through high-speed water adding emulsification, so that the stability of the self-made waterborne epoxy resin is obviously improved, and the solvent in the system is removed, so that the system is odorless and high in environmental protection performance; the two-component water-based epoxy coating can be adjusted into different colors, and can meet the requirements of interior decoration.
In one embodiment, the pigment and filler is one or more of titanium dioxide, calcined kaolin, talcum powder and calcium carbonate. Preferably, the titanium dioxide is rutile titanium dioxide with better covering power and aging resistance, such as R-706 produced by DuPont company.
In one embodiment, the particle size of the pigment and filler is 800-1500 meshes.
In one embodiment, the filler is a low oil absorption filler.
In one embodiment, the aqueous epoxy curing agent is Anquamine721, us air chemical and/or Aradur39, us huntsman. Anquamine721, Hensman Aradur39 are light in color, little or no odor, and have a broad range of ratios with aqueous epoxies.
In one embodiment, the auxiliary agent 1 is one or more of a defoaming agent, a thickening agent, a wetting agent and a dispersing agent.
In one embodiment, the auxiliary agent 1 is one or more of a defoaming agent, a thickening agent, a wetting agent and a dispersing agent.
The assistant 1 and the assistant 2 comprise but are not limited to water-based assistant systems such as basf, BYK and air chemical industry. According to actual use requirements and surface effects, the invention can preferably select an aqueous auxiliary agent, specifically a defoaming agent FOAMSTAR ST 2140AC, a dispersing agent BYK190, a wetting agent Surfynol 104E, a thickening agent PU 1190, Dow RM-8W and the like.
In one embodiment, the component A also contains water-based color paste. The color paste can be water-based color paste with various specifications which is already marketed.
In one embodiment, the preparation method of the water-based epoxy resin comprises the following steps:
s1, adding 160-plus 200 parts of epoxy resin E-44 into a reaction container, stirring and heating to 55 +/-5 ℃, adding 210-plus 250 parts of diisocyanate, and controlling the temperature to be 50-70 ℃ for heat preservation and reaction for 50-150 min;
s2, adding 40-50 parts of polycaprolactone with molecular weight of 1000-2000 and 30-50 parts of micromolecular dihydric alcohol into a reaction vessel, and preserving heat at 68 +/-2 ℃ for 60 +/-10 min;
s3, adding 30-40 parts of dimethylolbutyric acid, dropwise adding 2-5 drops of tin catalyst, and keeping the temperature at 68 +/-2 ℃ for 2 +/-0.5 hours;
s4, detecting the content of NCO in the system, when the content of NCO reaches 1.5-4.0%, adding 50-80 parts of epoxy resin E-51, preserving heat for 60 +/-10 min at 66-68 ℃, then heating to 75 +/-5 ℃, adding 10-20 parts of hydrogen peroxide, preserving heat for 60 +/-10 min, adding 300 portions of solvent, reducing viscosity and stirring for 10-30 min;
s5, cooling to 55 +/-5 ℃, sequentially adding 15-20 parts of caustic soda and 2-3 parts of nonionic emulsifier into a reaction container, stirring for 5-10min at a stirring speed of 500-1500 r/min, then increasing the stirring speed to 1300-1500r/min, rapidly adding pure water at 75 +/-5 ℃ into a four-neck flask, emulsifying for 1.5-2.5h at a temperature of 60 +/-2 ℃, vacuumizing for 1-2h to remove the solvent in the system, keeping the temperature at 55-60 ℃, measuring the solid content, stopping stirring when the solid content reaches 55-57%, and standing for 6-10h to obtain the anionic waterborne epoxy resin emulsion.
In one embodiment, the diisocyanate is one or more of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, and hexamethylene diisocyanate.
In one embodiment, step S1 is: s1, adding 160-200 parts of epoxy resin E-44 into a reaction container, adding 60-90 parts of toluene diisocyanate, heating to 60 ℃, keeping the temperature for 40min, then adding 120-160 parts of isophorone diisocyanate into the reaction container, dropwise adding 2-5 drops of bismuth isooctanoate, slowly and automatically heating to 68 +/-2 ℃, and keeping the temperature for 90 min.
In one embodiment, the small molecule diol is 1, 6-hexanediol and/or 1, 4-butanediol, preferably, the small molecule diol is 1, 6-hexanediol.
In one embodiment, the dimethylolbutyric acid of step S3 is dissolved in N, N-dimethylformamide prior to addition.
In one embodiment, the tin catalyst in step S3 is stannous octoate.
In one example, the epoxy resin E-44 was pretreated as follows before the experiment: and adding 0.5% of antioxidant and 0.5% of weak acid into the epoxy resin E-44, and vacuumizing for 3 hours for later use under the condition of introducing nitrogen at 100-105 ℃.
In one example, the polycaprolactone was pretreated before the experiment as follows: and vacuumizing polycaprolactone at 100-105 ℃ for 1 h.
In one embodiment, the nonionic emulsifier is a polyoxyethylene ether, which can improve the storage stability and the high shear emulsification stability of the emulsion.
In one embodiment, the solvent in steps S4 and S5 is acetone.
The preparation method of the two-component water-based epoxy coating comprises the following steps:
(1) stirring the raw materials of the component A at 1000-1200 rpm for 60-90 min, uniformly mixing, and filtering to obtain a component A;
(2) stirring the raw materials in the pulping stage of the component B at 600-800 rpm for 20-30 min, and filtering to obtain a component B;
(3) before coating, the component A and the component B are mixed according to the ratio of 1-2: 1 to obtain the double-component water-based epoxy coating.
The two-component water-based epoxy paint is applied to water-based epoxy wall paint. Preferably, the wall paint is an interior wall paint. The water-based epoxy coating can meet the requirement of interior decoration, can be used as water-based epoxy wall paint, has good stain resistance effect and strong isolation, and can meet the requirement of high-cleanness decoration.
The invention has the beneficial effects that: according to the invention, hydrophilic groups are introduced into a molecular chain by a prepolymer method, the prepolymer with epoxy groups at both ends of the molecular chain and at the end functional groups of the side chain is synthesized, salt is synthesized in caustic soda, and the hydrophilic groups extend to a water phase to wrap the epoxy groups in emulsion colloidal particles through high-speed water adding emulsification, so that the stability of the self-made waterborne epoxy resin is obviously improved, and the solvent in the system is removed, so that the system is odorless and high in environmental protection performance; the emulsion obtained by using caustic soda for neutralization and salt formation has better stability than triethylamine, and can avoid the phenomenon that the triethylamine promotes phenol groups of epoxy resin to form a quinoid structure to generate yellowing phenomenon; the two-component water-based epoxy paint is prepared by using the self-made water-based epoxy resin as a main film forming substance, the proportion of pigment and filler in the paint film is reasonably mixed, the paint film reacts with a water-based epoxy resin curing agent to form a compact physical paint film, the mercerizing, shell polishing and matte effects can be obtained, different colors can be adjusted, the requirement of indoor decoration can be met, the obtained two-component water-based epoxy paint can be used as a water-based epoxy wall paint, the stain resistance effect is good, the isolation performance is strong, and the high-cleanness decoration requirement can be met.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the detailed description and specific examples, while indicating the scope of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
The following examples used the raw materials epoxy resin E-44 (technical Nanbao resin), epoxy resin E-51 (technical Nanbao resin), isophorone diisocyanate (IPDI) (technical German Bayer), Toluene Diisocyanate (TDI) (technical German Basff), polycaprolactone diol (PC L) (Mn 1500/2000 technical Japan cellosolve, DMBA) (technical Swedish Pastout), 1, 6-Hexanediol (HDO) (technical Mitsubishi corporation), caustic soda (analytical Tianjin Body chemical industry), DMF (analytical pure Tianjin Body chemical industry), acetone (technical Shang, Nami Spongdi chemical industry), bismuth octoate (analytical pure Xisu scientific GmbH), self-made hydrogen peroxide (analytical Korea), hydrochloric acid (analytical pure Xiong Gangtang chemical industry), antioxidant BHT (industrial Qingdao Longqing chemical industry), stannous (analytical pure Xiong chemical Yongsu), non-ionic emulsifier (environmental friendly chemical industry Co., Ltd).
The epoxy resin E-44 was pretreated as follows before the experiment: and adding 0.5% of antioxidant and 0.5% of weak acid into the epoxy resin E-44, and vacuumizing for 3 hours for later use under the condition of introducing nitrogen at 100-105 ℃.
Before the experiment, the polycaprolactone is pretreated as follows: and vacuumizing polycaprolactone at 100-105 ℃ for 1 h.
The following examples measure the-NCO concentration as follows:
NCO%=(V1-V0)*C1*42*100/nM1
wherein V1 represents the volume of hydrochloric acid consumed in blank detection, V0 represents the volume of hydrochloric acid consumed in prepolymer detection, C1 represents the volume concentration of hydrochloric acid, n represents the mass fraction of prepolymer, and M1 represents the mass of sample to be detected.
The following examples measure solids content as follows:
weighing 1 +/-0.2 g of emulsion in a glass watch glass, putting the emulsion into an oven to be baked for 30min at 150 ℃, then taking out the emulsion to be put into a dry glass ware to be cooled for 10min, and then taking out the emulsion to weigh the mass, wherein the calculation formula of the solid content is as follows: wt ═ M1-M0)/M
Where M1 is the mass of the emulsion plus the petri dish after baking, M0 is the mass of the petri dish, and M is the mass of the initially weighed emulsion), the average of three replicates was determined as the solids content of the sample.
The waterborne epoxy resins I described in examples 1 to 4 were prepared as follows:
s1, adding 160 parts of epoxy resin E-44 into a four-neck flask, starting stirring, slowly heating to 55 ℃, stopping heating, adding 90 parts of TDI, automatically heating to 60 ℃, preserving heat for 40min, then adding 126.54 parts of IPDI into the four-neck flask, dropwise adding 3 drops of bismuth isooctanoate, slowly and automatically heating to 68 +/-2 ℃, and preserving heat for 90 min;
s2, adding 40 parts of PC L with the molecular weight of 1500-inch and 2000 parts of 1, 6-hexanediol into a four-neck flask, and preserving the temperature at 68 +/-2 ℃ for 60 min;
s3, adding 32 parts of DMBA dissolved by DMF, dropwise adding 3 drops of stannous octoate, and keeping the temperature at 68 +/-2 ℃ for 2 hours;
s4, detecting the content of NCO in a system by a di-n-butylamine method, adding 70 parts of epoxy resin E-51 when the content of NCO reaches 3.0-4.0%, preserving heat for 60min at 66-68 ℃, then heating to 75 ℃, adding 16 parts of hydrogen peroxide, preserving heat for 60min, adding 350 parts of acetone, reducing viscosity and stirring for 15 min;
s5, cooling to 55 ℃, sequentially adding 15 parts of caustic soda and 3 parts of nonionic emulsifier polyoxyethylene ether into a four-neck flask, stirring for 5-10min at a stirring speed of 500-700r/min, then increasing the stirring speed to 1300r/min, rapidly adding 75 ℃ pure water into the four-neck flask, emulsifying for 2h at the temperature of 60 +/-2 ℃, vacuumizing for 1-2h to remove acetone in the system, keeping the temperature at 55-60 ℃, measuring the solid content, stopping stirring when the solid content reaches 55-57%, and standing for 8h to obtain the anionic waterborne epoxy resin emulsion.
The waterborne epoxy resin II described in example 5 was prepared as follows:
s1, putting 190 parts of epoxy resin E-44 into a four-neck flask, starting stirring, slowly heating to 55 ℃, stopping heating, adding 90 parts of TDI, automatically heating to 60 ℃, preserving heat for 40min, then adding 160 parts of IPDI into the four-neck flask, dropwise adding 4 drops of bismuth isooctanoate, slowly and automatically heating to 68 +/-2 ℃, and preserving heat for 90 min;
s2, adding 50 parts of PC L with the molecular weight of 1500-inch and 2000 parts of 1, 6-hexanediol into a four-neck flask, and preserving the temperature for 60min at 68 +/-2 ℃;
s3, adding 38 parts of DMBA dissolved by DMF, dropwise adding 4 drops of stannous octoate, and keeping the temperature at 68 +/-2 ℃ for 2 hours;
s4, detecting the content of NCO in a system by a di-n-butylamine method, adding 52 parts of epoxy resin E-51 when the content of NCO reaches 3.5-4.0%, preserving heat for 60min at 66-68 ℃, then heating to 75 ℃, adding 19 parts of hydrogen peroxide, preserving heat for 60min, adding 350 parts of acetone, reducing viscosity and stirring for 15 min;
s5, cooling to 55 ℃, sequentially adding 18 parts of caustic soda and 2-3 parts of nonionic emulsifier polyoxyethylene ether into a four-neck flask, stirring for 5-10min at a stirring speed of 500-700r/min, then increasing the stirring speed to 1500r/min, rapidly adding 75 ℃ pure water into the four-neck flask, emulsifying for 2h at the temperature of 60 +/-2 ℃, vacuumizing for 1-2h to remove acetone in the system, keeping the temperature at 55-60 ℃, measuring the solid content, stopping stirring when the solid content reaches 55-57%, and standing for 8h to obtain the anionic waterborne epoxy resin emulsion.
The waterborne epoxy resin III described in example 6 was prepared as follows:
s1, adding 170 parts of epoxy resin E-44 into a four-neck flask, starting stirring, slowly heating to 55 ℃, stopping heating, adding 70 parts of TDI, automatically heating to 60 ℃, preserving heat for 40min, then adding 150 parts of IPDI into the four-neck flask, dropwise adding 3 drops of bismuth isooctanoate, slowly and automatically heating to 68 +/-2 ℃, and preserving heat for 90 min;
s2, adding 40 parts of PC L with the molecular weight of 1500-inch and 2000 parts of 1, 6-hexanediol into the four-neck flask, and preserving the temperature for 60min at 68 +/-2 ℃;
s3, adding 35 parts of DMBA dissolved by DMF, dripping 3 drops of stannous octoate, and keeping the temperature at 68 +/-2 ℃ for 2 hours;
s4, detecting the content of NCO in a system by a di-n-butylamine method, adding 75 parts of epoxy resin E-51 when the content of NCO reaches 1.8-2.45%, preserving heat for 60min at 66-68 ℃, then heating to 75 ℃, adding 10 parts of hydrogen peroxide, preserving heat for 60min, adding 350 parts of acetone, reducing viscosity and stirring for 15 min;
s5, cooling to 55 ℃, sequentially adding 15 parts of caustic soda and 2-3 parts of nonionic emulsifier polyoxyethylene ether into a four-neck flask, stirring for 5-10min at a stirring speed of 500-700r/min, then increasing the stirring speed to 1300r/min, rapidly adding 75 ℃ pure water into the four-neck flask, emulsifying for 2h at the temperature of 60 +/-2 ℃, vacuumizing for 1-2h to remove acetone in the system, keeping the temperature at 55-60 ℃, measuring the solid content, stopping stirring when the solid content reaches 55-57%, and standing for 8h to obtain the anionic waterborne epoxy resin emulsion.
Example 1
A double-component water-based epoxy interior wall coating comprises the following components in parts by weight:
component A
Figure BDA0001489429690000081
Adding deionized water into a dispersion kettle, adding the above materials while stirring, stirring and dispersing at 1200rpm until the fineness of the slurry is less than 30um, and normally dispersing for 60 min.
Component B
Figure BDA0001489429690000082
And (3) putting the materials into a material making kettle in sequence, adjusting the stirring speed to 800rpm, and stirring and dispersing for 30 min. Filtering and packaging to obtain 100 parts by mass of a component B of the two-component interior wall coating.
Before painting, the paint is coated according to the proportion of 1: 1, evenly mixing A, B components, adding A, B percent of water accounting for about 10 percent of the total weight of the mixture, and effectively dispersing for more than 2min to obtain the two-component water-based epoxy interior wall coating with good shell gloss, good stain resistance, excellent decorative effect, scrubbing resistance and good isolation.
Example 2
A double-component water-based epoxy interior wall coating comprises the following components in parts by weight:
component A
Figure BDA0001489429690000091
Adding deionized water into a dispersion kettle, adding the above materials while stirring, stirring and dispersing at 1200rpm until the fineness of the slurry is less than 30um, normally dispersing for 60min, and if color mixing is required, adding commercially available water-based color pastes with various specifications.
Component B
Figure BDA0001489429690000092
And (3) putting the materials into a material making kettle in sequence, adjusting the stirring speed to 800rpm, and stirring and dispersing for 30 min. Filtering and packaging to obtain 100 parts by mass of a component B of the two-component interior wall coating.
Before painting, the paint is coated according to the proportion of 1: 1, evenly mixing A, B components, adding A, B percent of water accounting for about 10 percent of the total weight of the mixture, and effectively dispersing for more than 2min to obtain the double-component water-based epoxy interior wall coating with excellent mercerization, stain resistance, decorative effect, scrubbing resistance and isolation.
Example 3
A double-component water-based epoxy interior wall coating comprises the following components in parts by weight:
the component A comprises:
Figure BDA0001489429690000101
adding deionized water into a dispersion kettle, adding the above materials while stirring, stirring and dispersing at 1000rpm until the fineness of the slurry is less than 30um, normally dispersing for 90min, and if color mixing is required, adding commercially available water-based color pastes with various specifications.
Component B
Figure BDA0001489429690000102
And (3) putting the materials into a material making kettle in sequence, adjusting the stirring speed to 600rpm, and stirring and dispersing for 20 min. Filtering and packaging to obtain 100 parts by mass of a component B of the two-component interior wall coating.
Before painting, A, B components are uniformly mixed according to the mass ratio of A to B being 2 to 1, then A, B percent of water with the total amount being about 10 percent is added, and the mixture is effectively dispersed for more than 2min, so that the two-component water-based epoxy interior wall coating with matte, good stain resistance, excellent decorative effect, scrubbing resistance and good isolation can be obtained.
Example 4
A double-component water-based epoxy interior wall coating comprises the following components in parts by weight:
component A
Figure BDA0001489429690000111
Adding deionized water into a dispersion kettle, adding the above materials while stirring, stirring and dispersing at 1200rpm until the fineness of the slurry is less than 30um, and normally dispersing for 60 min.
Component B
Figure BDA0001489429690000112
And (3) putting the materials into a material making kettle in sequence, adjusting the stirring speed to 800rpm, and stirring and dispersing for 30 min. Filtering and packaging to obtain 100 parts by mass of a component B of the two-component interior wall coating.
Before painting, the paint is coated according to the proportion of 1: 1, evenly mixing A, B components, adding A, B percent of water accounting for about 10 percent of the total weight of the mixture, and effectively dispersing for more than 2min to obtain the two-component water-based epoxy interior wall coating with bright light, good stain resistance, excellent decorative effect, scrubbing resistance and good isolation.
Example 5
A two-component water-based epoxy interior wall coating has basically the same composition and preparation method as those of example 1, and is different from the water-based epoxy resin used in the example, namely, the self-made water-based epoxy resin II is used in the example.
Example 6
A two-component water-based epoxy interior wall coating is basically the same as the coating in example 1 in composition and preparation method, and is different from the water-based epoxy resin used in the example, namely the self-made water-based epoxy resin III.
Comparative example 1
Kanghujia odor-free 100 wall paint produced by Jia Bao Li company.
Comparative example 2
The five-in-one interior wall finish with porcelain and pure flavor produced by Nippon company.
Comparative example 3
Water-based glaze finish paint produced by Suzhou Deda special coating company Limited.
The wall paint obtained in the examples 1-6 and the comparative examples 1-3 is subjected to a performance test, and the test method is as follows:
the texture of a paint film is as follows: visual inspection;
gloss: visual inspection;
water pen test stain resistance: painting on the wall paint with water-based white board pen, and wiping with wet rag dipped in water.
The test results are shown in Table 1.
TABLE 1
Figure BDA0001489429690000121
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (8)

1. The two-component water-based epoxy coating is characterized by comprising the following components in parts by mass:
the component A comprises:
Figure FDA0002388978060000011
the component B comprises:
10-40 parts by mass of deionized water;
20.8-2 parts by mass of an auxiliary agent;
50-90 parts by mass of self-made waterborne epoxy resin;
the preparation method of the self-made waterborne epoxy resin comprises the following steps:
s1, adding 160-plus 200 parts of epoxy resin E-44 into a reaction container, stirring and heating to 55 +/-5 ℃, adding 210-plus 250 parts of diisocyanate, and controlling the temperature to be 50-70 ℃ for heat preservation and reaction for 50-150 min;
s2, adding 40-50 parts of polycaprolactone with molecular weight of 1000-2000 and 30-50 parts of micromolecular dihydric alcohol into a reaction vessel, and preserving heat at 68 +/-2 ℃ for 60 +/-10 min;
s3, adding 30-40 parts of dimethylolbutyric acid, dropwise adding 2-5 drops of tin catalyst, and keeping the temperature at 68 +/-2 ℃ for 2 +/-0.5 hours;
s4, detecting the content of NCO in the system, when the content of NCO reaches 1.5-4.0%, adding 50-80 parts of epoxy resin E-51, preserving heat for 60 +/-10 min at 66-68 ℃, then heating to 75 +/-5 ℃, adding 10-20 parts of hydrogen peroxide, preserving heat for 60 +/-10 min, adding 300 portions of solvent, reducing viscosity and stirring for 10-30 min;
s5, cooling to 55 +/-5 ℃, sequentially adding 15-20 parts of caustic soda and 2-3 parts of nonionic emulsifier into a reaction container, stirring for 5-10min at a stirring speed of 500-1500 r/min, then increasing the stirring speed to 1300-1500r/min, rapidly adding pure water at 75 +/-5 ℃ into a four-neck flask, emulsifying for 1.5-2.5h at a temperature of 60 +/-2 ℃, vacuumizing for 1-2h to remove the solvent in the system, keeping the temperature at 55-60 ℃, measuring the solid content, stopping stirring when the solid content reaches 55-57%, and standing for 6-10h to obtain the anionic waterborne epoxy resin emulsion.
2. The two-component waterborne epoxy coating of claim 1, wherein the pigment and filler is one or more of titanium dioxide, calcined kaolin, talc and calcium carbonate.
3. The two-component water-based epoxy coating as claimed in claim 2, wherein the pigment filler has a particle size of 800-1500 meshes.
4. The two-component water-based epoxy coating according to claim 1, wherein the water-based epoxy curing agent is Anquamine721 of American air chemical and/or Aradur39 of American Hounsfield.
5. The two-component water-based epoxy coating material as claimed in claim 1, wherein the auxiliary agent 1 is one or more of a defoaming agent, a thickening agent, a wetting agent and a dispersing agent.
6. The two-component water-based epoxy coating material as claimed in claim 1, wherein the auxiliary agent 2 is one or more of a defoaming agent, a thickening agent, a wetting agent and a dispersing agent.
7. The method for preparing the two-component water-based epoxy coating material according to any one of claims 1 to 6, comprising the steps of:
(1) stirring the raw materials of the component A at 1000-1200 rpm for 60-90 min, uniformly mixing, and filtering to obtain a component A;
(2) stirring the raw materials in the pulping stage of the component B at 600-800 rpm for 20-30 min, and filtering to obtain a component B;
(3) before coating, the component A and the component B are mixed according to the ratio of 1-2: 1 to obtain the double-component water-based epoxy coating.
8. The use of the two-component waterborne epoxy coating of any one of claims 1-6 in a waterborne epoxy wall finish.
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