CN115594864A - Water-based epoxy emulsion, high-film-thickness epoxy primer and preparation method thereof - Google Patents
Water-based epoxy emulsion, high-film-thickness epoxy primer and preparation method thereof Download PDFInfo
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- CN115594864A CN115594864A CN202211171486.6A CN202211171486A CN115594864A CN 115594864 A CN115594864 A CN 115594864A CN 202211171486 A CN202211171486 A CN 202211171486A CN 115594864 A CN115594864 A CN 115594864A
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- 239000004593 Epoxy Substances 0.000 title claims abstract description 153
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 110
- 239000000839 emulsion Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title abstract description 24
- 239000003822 epoxy resin Substances 0.000 claims abstract description 103
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 103
- 239000006184 cosolvent Substances 0.000 claims abstract description 56
- ARXJGSRGQADJSQ-UHFFFAOYSA-N 1-methoxypropan-2-ol Chemical compound COCC(C)O ARXJGSRGQADJSQ-UHFFFAOYSA-N 0.000 claims abstract description 52
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 38
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 claims abstract description 36
- 239000002270 dispersing agent Substances 0.000 claims abstract description 34
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 22
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 18
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000049 pigment Substances 0.000 claims abstract description 16
- 239000002562 thickening agent Substances 0.000 claims abstract description 16
- 238000009736 wetting Methods 0.000 claims abstract description 16
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000006229 carbon black Substances 0.000 claims abstract description 15
- 235000010215 titanium dioxide Nutrition 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims description 98
- 238000006243 chemical reaction Methods 0.000 claims description 24
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 21
- 238000005576 amination reaction Methods 0.000 claims description 18
- 239000011268 mixed slurry Substances 0.000 claims description 16
- 238000005303 weighing Methods 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 14
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 239000007787 solid Substances 0.000 claims description 7
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 2
- 230000031877 prophase Effects 0.000 claims description 2
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 2
- 229940043237 diethanolamine Drugs 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 15
- 239000003973 paint Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 4
- 238000005336 cracking Methods 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 125000003277 amino group Chemical group 0.000 description 2
- 239000012752 auxiliary agent Substances 0.000 description 2
- 125000003700 epoxy group Chemical group 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical group [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000007888 film coating Substances 0.000 description 1
- 238000009501 film coating Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000019832 sodium triphosphate Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- UNXRWKVEANCORM-UHFFFAOYSA-I triphosphate(5-) Chemical compound [O-]P([O-])(=O)OP([O-])(=O)OP([O-])([O-])=O UNXRWKVEANCORM-UHFFFAOYSA-I 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates 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
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
-
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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
- C09D5/002—Priming paints
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G2150/00—Compositions for coatings
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2363/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2463/00—Characterised by the use of epoxy resins; Derivatives of epoxy resins
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- Chemical & Material Sciences (AREA)
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- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
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Abstract
A waterborne epoxy emulsion, high film thickness epoxy primer and its preparation method, in the field of waterborne coating processing technology, a waterborne epoxy emulsion, by weight, includes 1-2 parts of epoxy component A, 43-50 parts of epoxy resin B, 6-8 parts of cosolvent B, 4-6 parts of emulsifier, 0.1-0.2 part of dispersant, 35-40 parts of water, 0.2-0.3 part of epoxy resin C; the high-film-thickness epoxy primer comprises the following components in percentage by mass of 6-8:1, wherein the component A comprises the following components in parts by weight: 35-45 parts of water-based epoxy emulsion, 1-2 parts of propylene glycol methyl ether, 0.1-0.2 part of defoaming agent, 0.4-0.5 part of dispersing agent, 0.1-0.2 part of wetting and leveling agent, 0.5-1 part of anti-flash rust agent, 0.1-0.2 part of montmorillonite clay, 0.3-0.5 part of dipropylene glycol butyl ether, 5-8 parts of antirust pigment, 3-5 parts of titanium white, 0.1-0.2 part of carbon black, 20-23 parts of barium sulfate, 24-27 parts of water A, 0.3-0.5 part of thickening agent, and the component B comprises: 45-50 parts of epoxy curing agent, 10-15 parts of propylene glycol monomethyl ether and 45-50 parts of water B. The limit film thickness of the high-film-thickness epoxy primer prepared by the water-based epoxy emulsion is more than 200 mu m.
Description
Technical Field
The invention belongs to the technical field of water-based paint processing, and particularly relates to a water-based epoxy emulsion, a high-film-thickness epoxy primer and a preparation method thereof.
Background
The use of aqueous epoxy two-component materials has become an indispensable product in industrial paint applications, and the properties of aqueous epoxy two-component materials are diversified and can meet the diversity of market requirements.
In the practical application process, the epoxy double-component is generally only used as a primer, the used film thickness has certain limitation, but for some special products, such as a sanitary clean room and a factory building, a highly corrosive animal husbandry building, a chemical building with a strong corrosive atmosphere and the like, the aging and the peeling of the coating can be accelerated due to a high corrosive environment or severe weather, the high-film-thickness coating is needed, the high-film-thickness primer film coating is improved, but the limit film thickness of the existing epoxy water-based paint is only about 80 μm, and the surface cracking can occur when the limit film thickness is exceeded.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a water-based epoxy emulsion, a high-film-thickness epoxy primer and a preparation method thereof. The limit film thickness of the formed paint film of the high-film-thickness epoxy primer prepared by the water-based epoxy emulsion can reach more than 200 mu m.
The invention adopts the specific technical scheme that:
the water-based epoxy emulsion comprises the following components in parts by weight: 1-2 parts of epoxy component A, 43-50 parts of epoxy resin B, 6-8 parts of cosolvent B, 4-6 parts of emulsifier, 0.1-0.2 part of dispersant, 35-40 parts of water and 0.2-0.3 part of epoxy resin C;
the epoxy component A consists of the following components in percentage by weight: 62-68% of epoxy resin A, 15-22% of cosolvent A and 14-20% of diethanolamine;
the epoxy resin A is solid epoxy resin, and the epoxy equivalent is 450-1000g/eq;
the epoxy resin B is solid epoxy resin, and the epoxy equivalent is 450-1000g/eq;
the epoxy resin C is liquid epoxy resin, and the epoxy equivalent is 180-190g/eq.
Furthermore, the cosolvent A is an alcohol ether cosolvent, the alcohol ether cosolvent is one or two of ethylene glycol butyl ether and propylene glycol methyl ether, and the cosolvent B and the cosolvent A have the same components.
The high-film-thickness epoxy primer comprises a water-based epoxy emulsion, and consists of a component A and a component B, wherein the mass ratio of the component A to the component B is (6-8): 1;
wherein the component A comprises the following components in parts by weight: 35-45 parts of water-based epoxy emulsion, 1-2 parts of propylene glycol methyl ether, 0.1-0.2 part of defoaming agent, 0.4-0.5 part of dispersant, 0.1-0.2 part of wetting leveling agent, 0.5-1 part of anti-flash rust agent, 0.1-0.2 part of montmorillonite clay, 0.3-0.5 part of dipropylene glycol butyl ether, 5-8 parts of antirust pigment, 3-5 parts of titanium white, 0.1-0.2 part of carbon black, 20-23 parts of barium sulfate, 24-27 parts of water A and 0.3-0.5 part of thickener;
the component B comprises the following components in parts by weight: 45-50 parts of epoxy curing agent, 10-15 parts of propylene glycol monomethyl ether and 45-50 parts of water B.
A preparation method of the high-film-thickness epoxy primer comprises the following steps:
a: preparing a water-based epoxy emulsion;
b: weighing the components according to the proportion of the high-film-thickness epoxy primer for later use;
c: adding water A, 40-60% of the content of the defoaming agent, a dispersing agent and propylene glycol methyl ether into a container, uniformly stirring, adding montmorillonite clay, dipropylene glycol butyl ether, an anti-rust pigment, carbon black, titanium white and barium sulfate, uniformly stirring to obtain a mixed slurry, and grinding the mixed slurry to the fineness of less than or equal to 25 mu m to obtain a prophase slurry;
d: c, adding the water-based epoxy emulsion, the dipropylene glycol butyl ether, the early-stage slurry obtained in the step C, the wetting and leveling agent and the rest defoaming agent into another container, uniformly stirring, adding the thickening agent, and uniformly stirring to obtain a component A;
e: and (3) uniformly mixing the epoxy curing agent and propylene glycol monomethyl ether, adding water B, and uniformly stirring to obtain the component B.
Further, the preparation of the aqueous epoxy emulsion in the step A comprises the following steps:
a1: weighing the components according to the proportion of the water-based epoxy emulsion for later use;
a2: pouring the epoxy resin A and the cosolvent A into a container, heating until the epoxy resin A is completely melted, adding diethanolamine into the container, and aminating to obtain an epoxy component A;
a3: and (3) adding the epoxy resin B, the cosolvent B and the emulsifier into another container, heating until the epoxy resin B is completely melted, then sequentially adding the dispersant, 30-40% of the total amount of water, 30-40% of the epoxy component A obtained in the step A2, and the rest water, stirring after adding the components each time, adding the epoxy resin C, stirring in a heating and heat-preserving state, and filtering to obtain the water-based epoxy emulsion.
Further, adding diethanolamine into the step A2, and reacting at 115-125 ℃ for 1.5-2.5h for amination.
Further, the stirring in the heating and heat preservation state in the step A3 is stirring for 2-4h at the rotating speed of 500-800r/min at the temperature of 85-95 ℃.
Further, the step C of uniformly stirring to obtain mixed slurry is to stir for 15-20 min at 700-800 r/min.
And further, adding water B in the step E, and stirring uniformly at 400-500 r/min for 10-20min.
The invention has the beneficial effects that:
1. the limit film thickness of the prepared high-film-thickness primer is more than 200 mu m, solid epoxy resin A accounting for 1-2% of the total mass of the water-based epoxy emulsion is aminated to change the molecular structure of the primer, the molecular structure of the primer contains amino, the epoxy resin A is sequentially fused with solid epoxy resin B, water and other additives according to a specific sequence, the epoxy resin A with the amino is uniformly dispersed to each corner of an emulsion system, the emulsion system obtains better elongation at break, the limit film thickness is improved, only 1-2% of the solid epoxy resin is aminated because the excessive amination of the epoxy resin of the system can cause the system hardness to be too large and the curing speed to be too high, so that the surface of a paint film is easy to crack, and finally, the liquid epoxy resin is added into the emulsion system, so that fine granular resin colloidal particles can be generated by adding the liquid epoxy resin, the resin colloidal particles have better viscosity, the viscosity of the system can be increased while the film thickness is improved, and the occurrence of the cracking situation is reduced, so that the limit film thickness of the epoxy primer is further improved.
2. The waterborne epoxy emulsion has enough viscosity and rheological property, so that the addition amount of barium sulfate is reduced in the process of preparing the epoxy primer with high film thickness, the condition that the surface of a paint film cracks due to excessive barium sulfate is avoided, the cost is reduced, and the content of heavy metal in the epoxy primer is reduced.
3. In the invention, when amination is carried out in the preparation process of the aqueous epoxy emulsion, the equivalent ratio of the epoxy resin A to the diethanol amine is less than or equal to 1:2, namely, diethanolamine is excessive by 1 time, so that the epoxy resin A can be fully aminated, the amination is more thorough, and the formed epoxy resin condensate has higher strength and elongation at break, so that the surface of the prepared high-film-thickness epoxy primer is not easy to crack, the limiting film thickness is higher, and the amination is carried out at 115-125 ℃ so as to excite the activity of the amino group and the epoxy group and improve the curing speed of the amino group and the epoxy group.
4. In the invention, the components of the high-film-thickness epoxy primer contain a small amount of montmorillonite clay, and the montmorillonite clay has excellent characteristics of high dispersibility, adsorptivity, cohesiveness and the like, so that the high-film-thickness epoxy primer can be bonded with a part to be coated more tightly.
5. The stirring speed and the stirring time of the preparation method are limited, when the stirring speed is too low, the paint liquid is not easy to disperse, the agglomeration and coarseness are easy to generate, and when the stirring speed is too high, the demulsification in the aspect of product emulsion is easy to cause, the stirring time is to ensure that all components are fully and uniformly mixed, the effects of an auxiliary agent, a thickening agent and the like are optimal, when the stirring time is too short, the stirring is not uniform, when the stirring time is too long, the product temperature is higher, part of the auxiliary agent is volatilized, and by limiting the stirring speed and the stirring time of the preparation method, the adverse effect on the final performance of the product caused by the preparation process is avoided, so that the stability of the comprehensive performance of the product is provided.
Detailed Description
According to the invention, the epoxy resin A, the epoxy resin B and the epoxy resin C are 904 epoxy resin, 901 epoxy resin and 128 liquid epoxy resin which are respectively produced in Taiwan southern Asia, the emulsion is Nanjing Xinyi synthetic emulsifier 8910, the dispersant is American Zhanxin Allnex6208 dispersant, the wetting leveling agent is a rheological powder assistant which is produced by Hamming German moded company, the anti-flash rust agent is Defors T750 of Hofmann chemical company, the anti-rust pigment is modified aluminum tripolyphosphate which is produced by Hunan Ruishi stone scientific and technological development Co., ltd, the epoxy curing agent is AQUAUA-3126 which is produced by Jiangsu Fuqisen New Material Co., ltd, the mesh number of barium sulfate is 1500, the water A and the water B are deionized water, and other used raw materials can be purchased from the market if no special description exists.
1. Detailed description of the preferred embodiments
Example 1
Preparation of aqueous epoxy emulsions
A1: weighing 1.5 parts of epoxy component A, 46 parts of epoxy resin B, 7 parts of cosolvent B, 5 parts of emulsifier, 0.15 part of dispersant, 38 parts of water and 0.24 part of epoxy resin C,
wherein the epoxy component A consists of 65 percent of epoxy resin A, 20 percent of cosolvent A and 15 percent of diethanol amine by weight percentage,
wherein the cosolvent A and the cosolvent B are ethylene glycol butyl ether;
a2: pouring the epoxy resin A and the cosolvent A into a reaction kettle, heating to 145 ℃, cooling to 120 ℃ after the epoxy resin A is completely melted, adding diethanolamine to the mixture at the temperature of 120 ℃ for amination for 2h, wherein the equivalent ratio of the epoxy resin A to the diethanolamine is 1:2, obtaining an epoxy component A after amination;
a3: and (2) adding epoxy resin B, cosolvent B and emulsifier into another reaction kettle, heating to 115 ℃, adding a dispersant into the reaction kettle, stirring for 10min at 2000r/min after the epoxy resin B is completely melted, adding 35% of the total amount of water into the reaction kettle, stirring for 30min at 2000r/min, adding the epoxy component A obtained in the step A2, stirring for 5min at 2000r/min, adding 35% of the total amount of water, stirring for 20min at 2000r/min, adding the rest water, stirring for 30min at 2000r/min, adding epoxy resin C, stirring for 3h at 90 ℃ at 600r/min, and filtering to obtain the water-based epoxy emulsion.
Preparation of high-film-thickness epoxy primer
B: weighing the following components in a mass ratio of 7:1, component A and component B are ready for use,
wherein the component A comprises the following components in parts by weight: 40 parts of water-based epoxy emulsion, 1.4 parts of propylene glycol methyl ether, 0.15 part of defoaming agent, 0.45 part of dispersing agent, 0.13 part of wetting and leveling agent, 0.8 part of flash rust inhibitor, 0.15 part of montmorillonite clay, 0.4 part of dipropylene glycol butyl ether, 6 parts of rust-proof pigment, 4 parts of titanium white, 0.12 part of carbon black, 22 parts of barium sulfate, 25 parts of water A and 0.4 part of thickening agent,
the component B comprises the following components in parts by weight: 48 parts of epoxy curing agent, 13 parts of propylene glycol monomethyl ether and 48 parts of water B;
c: adding water A, 50% of the content of the defoaming agent, a dispersing agent and propylene glycol methyl ether into a stirrer, stirring for 10min at a speed of 500r/min, adding montmorillonite clay, dipropylene glycol butyl ether, an anti-rust pigment, carbon black, titanium white and barium sulfate, stirring for 18min at a speed of 750r/min to obtain mixed slurry, and grinding the mixed slurry until the fineness is less than or equal to 25 mu m to obtain early-stage slurry;
d: c, adding the water-based epoxy emulsion, the dipropylene glycol butyl ether, the early-stage slurry obtained in the step C, the wetting and leveling agent and the residual defoaming agent into another stirrer, stirring and mixing for 15min at the speed of 450r/min, adding the thickening agent, and uniformly stirring to obtain a component A;
e: stirring the epoxy curing agent and the propylene glycol monomethyl ether at 500r/min for 10min, adding the water B, and stirring at 600r/min for 15min to obtain the component B.
Example 2
Preparation of aqueous epoxy emulsions
A1: weighing 1 part of epoxy component A, 50 parts of epoxy resin B, 8 parts of cosolvent B, 4 parts of emulsifier, 0.2 part of dispersant, 40 parts of water and 0.3 part of epoxy resin C,
wherein the epoxy component A consists of 62 percent of epoxy resin A, 22 percent of cosolvent A and 16 percent of diethanol amine by weight percentage,
wherein the cosolvent A and the cosolvent B are propylene glycol monomethyl ether;
a2: pouring the epoxy resin A and the cosolvent A into a reaction kettle, heating to 150 ℃, cooling to 115 ℃ after the epoxy resin A is completely melted, adding diethanolamine to the mixture at the temperature of 115 ℃ for amination for 2.5h, wherein the equivalent ratio of the epoxy resin A to the diethanolamine is 1:2.2, obtaining an epoxy component A after amination;
a3: and (2) adding epoxy resin B, cosolvent B and an emulsifier into another reaction kettle, heating to 110 ℃, adding a dispersant into the reaction kettle, stirring for 12min at 2000r/min after the epoxy resin B is completely melted, adding 30% of the total amount of water, stirring for 25min at 2000r/min, adding the epoxy component A obtained in the step A2, stirring for 6min at 2000r/min, adding 40% of the total amount of water, stirring for 25min at 2000r/min, adding the rest water, stirring for 25min at 2000r/min, adding epoxy resin C, stirring for 2h at 800r/min at 85 ℃, and filtering to obtain the water-based epoxy emulsion.
Preparation of high-film-thickness epoxy primer
B: weighing 6:1, component A and component B are ready for use,
wherein the component A comprises the following components in parts by weight: 35 parts of water-based epoxy emulsion, 1 part of propylene glycol methyl ether, 0.1 part of defoaming agent, 0.5 part of dispersing agent, 0.1 part of wetting and leveling agent, 1 part of flash rust inhibitor, 0.1 part of montmorillonite clay, 0.5 part of dipropylene glycol butyl ether, 8 parts of antirust pigment, 5 parts of titanium white, 0.2 part of carbon black, 23 parts of barium sulfate, 24 parts of water A and 0.5 part of thickening agent,
the component B comprises the following components in parts by weight: 45 parts of epoxy curing agent, 10 parts of propylene glycol monomethyl ether and 50 parts of water B;
c: adding water A, 40% of the content of the defoaming agent, a dispersing agent and propylene glycol methyl ether into a stirrer, stirring for 12min at a speed of 400r/min, adding montmorillonite clay, dipropylene glycol butyl ether, an anti-rust pigment, carbon black, titanium white and barium sulfate, stirring for 20min at a speed of 700r/min to obtain mixed slurry, and grinding the mixed slurry until the fineness is less than or equal to 25 mu m to obtain early-stage slurry;
d: c, adding the water-based epoxy emulsion, the dipropylene glycol butyl ether, the early-stage slurry obtained in the step C, the wetting and leveling agent and the rest defoaming agent into another stirrer, stirring and mixing for 20min at a speed of 400r/min, adding the thickening agent, and uniformly stirring to obtain a component A;
e: stirring the epoxy curing agent and the propylene glycol monomethyl ether at 450r/min for 14min, adding the water B, and stirring at 500r/min for 10min to obtain the component B.
Example 3
Preparation of aqueous epoxy emulsions
A1: weighing 2 parts of epoxy component A, 43 parts of epoxy resin B, 6 parts of cosolvent B, 6 parts of emulsifier, 0.1 part of dispersant, 35 parts of water and 0.2 part of epoxy resin C,
wherein the epoxy component A consists of 68 percent of epoxy resin A, 15 percent of cosolvent A and 17 percent of diethanol amine by weight percentage,
wherein the cosolvent A and the cosolvent B are ethylene glycol butyl ether;
a2: pouring the epoxy resin A and the cosolvent A into a reaction kettle, heating to 145 ℃, cooling to 125 ℃ after the epoxy resin A is completely melted, adding diethanolamine to the reaction kettle at 125 ℃ for amination for 1.5h, wherein the equivalent ratio of the epoxy resin A to the diethanolamine is 1:2, obtaining an epoxy component A after amination;
a3: and (2) adding epoxy resin B, cosolvent B and an emulsifier into another reaction kettle, heating to 120 ℃, adding a dispersant into the reaction kettle, stirring for 10min at 2000r/min after the epoxy resin B is completely melted, adding 40% of the total amount of water into the reaction kettle, stirring for 20min at 2000r/min, adding the epoxy component A obtained in the step A2, stirring for 5min at 2000r/min, adding 30% of the total amount of water, stirring for 15min at 2000r/min, adding the rest water, stirring for 20min at 2000r/min, adding epoxy resin C, stirring for 2h at 500r/min at 95 ℃, and filtering to obtain the water-based epoxy emulsion.
Preparation of high-film-thickness epoxy primer
B: weighing 8 parts of: 1, component A and component B are ready for use,
wherein the component A comprises the following components in parts by weight: 45 parts of water-based epoxy emulsion, 2 parts of propylene glycol methyl ether, 0.2 part of defoaming agent, 0.4 part of dispersing agent, 0.2 part of wetting and leveling agent, 0.5 part of flash rust inhibitor, 0.2 part of montmorillonite clay, 0.3 part of dipropylene glycol butyl ether, 5 parts of antirust pigment, 3 parts of titanium white, 0.1 part of carbon black, 20 parts of barium sulfate, 27 parts of water A and 0.3 part of thickening agent,
the component B comprises the following components in parts by weight: 50 parts of epoxy curing agent, 15 parts of propylene glycol monomethyl ether and 45 parts of water B;
c: adding water A, 60% of the content of the defoaming agent, a dispersing agent and propylene glycol methyl ether into a stirrer, stirring for 8min at a speed of 500r/min, adding montmorillonite clay, dipropylene glycol butyl ether, an anti-rust pigment, carbon black, titanium white and barium sulfate, stirring for 15min at a speed of 800r/min to obtain mixed slurry, and grinding the mixed slurry until the fineness is less than or equal to 25 mu m to obtain early-stage slurry;
d: c, adding the water-based epoxy emulsion, the dipropylene glycol butyl ether, the early-stage slurry obtained in the step C, the wetting and leveling agent and the rest defoaming agent into another stirrer, stirring and mixing at 500r/min for 15min, adding the thickening agent, and uniformly stirring to obtain a component A;
e: stirring the epoxy curing agent and the propylene glycol monomethyl ether at 500r/min for 10min, adding the water B, and stirring at 400r/min for 20min to obtain the component B.
Example 4
Preparation of aqueous epoxy emulsion
A1: weighing 1.5 parts of epoxy component A, 45 parts of epoxy resin B, 5 parts of cosolvent B, 6 parts of emulsifier, 0.15 part of dispersant, 38 parts of water and 0.3 part of epoxy resin C,
wherein the epoxy component A consists of 64 percent of epoxy resin A, 16 percent of cosolvent A and 20 percent of diethanol amine by weight percentage,
wherein the cosolvent A and the cosolvent B are respectively a mixture of 1:1, a mixed cosolvent of ethylene glycol butyl ether and propylene glycol methyl ether;
a2: pouring the epoxy resin A and the cosolvent A into a reaction kettle, heating to 148 ℃, cooling to 122 ℃ after the epoxy resin A is completely melted, adding diethanolamine to the mixture at the temperature of 122 ℃ for amination for 1.8h, wherein the equivalent ratio of the epoxy resin A to the diethanolamine is 1:2.1, obtaining an epoxy component A after amination;
a3: and (2) adding the epoxy resin B, the cosolvent B and the emulsifier into another reaction kettle, heating to 110 ℃, adding the dispersant to stir at 2000r/min for 8min after the epoxy resin B is completely melted, adding 35% of the total water to stir at 2000r/min for 15min, adding the epoxy component A obtained in the step A2 to stir at 2000r/min for 6min, adding 30% of the total water to stir at 2000r/min for 15min, adding the rest water to stir at 2000r/min for 25min, adding the epoxy resin C to stir at 750r/min at 92 ℃ for 2.5h, and filtering to obtain the water-based epoxy emulsion.
Preparation of high-film-thickness epoxy primer
B: weighing the following components in a mass ratio of 7:1, component A and component B are ready for use,
wherein the component A comprises the following components in parts by weight: 42 parts of water-based epoxy emulsion, 1.6 parts of propylene glycol methyl ether, 0.16 part of defoaming agent, 0.48 part of dispersing agent, 0.15 part of wetting leveling agent, 0.8 part of anti-flash rust agent, 0.14 part of montmorillonite clay, 0.38 part of dipropylene glycol butyl ether, 7 parts of anti-rust pigment, 4 parts of titanium white, 0.18 part of carbon black, 21 parts of barium sulfate, 25 parts of water A and 0.35 part of thickening agent,
the component B comprises the following components in parts by weight: 47 parts of epoxy curing agent, 13 parts of propylene glycol monomethyl ether and 50 parts of water B;
c: adding water A, 50% of the content of the defoaming agent, a dispersing agent and propylene glycol methyl ether into a stirrer, stirring for 5min at a speed of 600r/min, adding montmorillonite clay, dipropylene glycol butyl ether, an anti-rust pigment, carbon black, titanium white and barium sulfate, stirring for 20min at a speed of 750r/min to obtain mixed slurry, and grinding the mixed slurry until the fineness is less than or equal to 25 mu m to obtain early-stage slurry;
d: c, adding the water-based epoxy emulsion, the dipropylene glycol butyl ether, the early-stage slurry obtained in the step C, the wetting and leveling agent and the rest defoaming agent into another stirrer, stirring and mixing for 15min at a speed of 450r/min, adding the thickening agent, and uniformly stirring to obtain a component A;
e: stirring an epoxy curing agent and propylene glycol monomethyl ether at 500r/min for 12min, adding water B, and stirring at 400r/min for 18min to obtain a component B.
Example 5
Preparation of aqueous epoxy emulsions
A1: weighing 1.8 parts of epoxy component A, 44 parts of epoxy resin B, 5 parts of cosolvent B, 5 parts of emulsifier, 0.1 part of dispersant, 40 parts of water and 0.3 part of epoxy resin C,
wherein the epoxy component A consists of 66 percent of epoxy resin A, 20 percent of cosolvent A and 14 percent of diethanol amine by weight percentage,
wherein the cosolvent A and the cosolvent B are ethylene glycol butyl ether;
a2: pouring the epoxy resin A and the cosolvent A into a reaction kettle, heating to 145 ℃, cooling to 120 ℃ after the epoxy resin A is completely melted, adding diethanolamine to the reaction kettle at 120 ℃ for amination for 2 hours, wherein the equivalent ratio of the epoxy resin A to the diethanolamine is 1:2, amination to obtain an epoxy component A;
a3: and (2) adding epoxy resin B, cosolvent B and emulsifier into another reaction kettle, heating to 115 ℃, adding a dispersant into the reaction kettle, stirring for 10min at 2000r/min after the epoxy resin B is completely melted, adding 35% of the total amount of water into the reaction kettle, stirring for 15min at 2000r/min, adding the epoxy component A obtained in the step A2, stirring for 5min at 2000r/min, adding 30% of the total amount of water, stirring for 15min at 2000r/min, adding the rest water, stirring for 25min at 2000r/min, adding epoxy resin C, stirring for 3h at 700r/min at 95 ℃, and filtering to obtain the water-based epoxy emulsion.
Preparation of high-film-thickness epoxy primer
B: weighing the components in a mass ratio of 7:1, component A and component B are ready for use,
wherein the component A comprises the following components in parts by weight: 44 parts of water-based epoxy emulsion, 1 part of propylene glycol methyl ether, 0.15 part of defoaming agent, 0.5 part of dispersing agent, 0.2 part of wetting and leveling agent, 1 part of anti-flash rust agent, 0.2 part of montmorillonite clay, 0.4 part of dipropylene glycol butyl ether, 8 parts of anti-rust pigment, 3 parts of titanium white, 0.1 part of carbon black, 23 parts of barium sulfate, 26 parts of water A and 0.4 part of thickening agent,
the component B comprises the following components in parts by weight: 45 parts of epoxy curing agent, 12 parts of propylene glycol monomethyl ether and 48 parts of water B;
c: adding water A, 45% of the content of the defoaming agent, a dispersing agent and propylene glycol methyl ether into a stirrer, stirring for 10min at a speed of 500r/min, adding montmorillonite clay, dipropylene glycol butyl ether, an anti-rust pigment, carbon black, titanium white and barium sulfate, stirring for 15min at a speed of 700r/min to obtain mixed slurry, and grinding the mixed slurry until the fineness is less than or equal to 25 mu m to obtain early-stage slurry;
d: c, adding the water-based epoxy emulsion, the dipropylene glycol butyl ether, the early-stage slurry obtained in the step C, the wetting and leveling agent and the residual defoaming agent into another stirrer, stirring and mixing at 500r/min for 12min, adding the thickening agent, and uniformly stirring to obtain a component A;
e: stirring the epoxy curing agent and the propylene glycol monomethyl ether at 500r/min for 10min, adding the water B, and stirring at 500r/min for 15min to obtain the component B.
Comparative example 1
Comparative example 1 differs from example 1 only in that the aqueous epoxy emulsion in comparative example 1 does not contain epoxy component a.
Comparative example 2
Comparative example 2 differs from example 1 only in that the aqueous epoxy emulsion in comparative example 2 does not contain epoxy resin C.
Comparative example 3
Preparation of aqueous epoxy emulsions
A1: weighing 1.5 parts of epoxy component A, 46 parts of epoxy resin B, 7 parts of cosolvent B, 5 parts of emulsifier, 0.15 part of dispersant, 38 parts of water and 0.24 part of epoxy resin C,
wherein the epoxy component A consists of 76 percent of epoxy resin A and 34 percent of cosolvent A by weight percentage,
wherein the cosolvent A and the cosolvent B are ethylene glycol butyl ether;
a2: pouring the epoxy resin A and the cosolvent A into a reaction kettle, heating to 145 ℃, and heating until the epoxy resin A is completely melted to obtain an epoxy component A;
a3: and (2) adding epoxy resin B, cosolvent B and emulsifier into another reaction kettle, heating to 115 ℃, adding a dispersant into the reaction kettle, stirring for 10min at 2000r/min after the epoxy resin B is completely melted, adding 35% of the total amount of water into the reaction kettle, stirring for 30min at 2000r/min, adding the epoxy component A obtained in the step A2, stirring for 5min at 2000r/min, adding 35% of the total amount of water, stirring for 20min at 2000r/min, adding the rest water, stirring for 30min at 2000r/min, adding epoxy resin C, stirring for 3h at 90 ℃ at 600r/min, and filtering to obtain the water-based epoxy emulsion.
Comparative example 3 differs from example 1 only in that the epoxy resin a in comparative example 3 was not aminated and the other preparation process of the high-film-thickness epoxy primer was the same as in example 1.
2. Performance testing
The component A and the component B prepared in the examples and the comparative examples are uniformly stirred and smeared within 30min, the performance of the obtained paint films is compared, the performance test results are shown in tables 1-2, and the appearance, gloss, flexibility, impact strength, adhesion, pencil hardness, water resistance and salt spray resistance tests are performed according to the industrial standard HG/T4758-2014; the limit film thickness test is carried out according to the national standard GB/T13452.2-92.
TABLE 1
TABLE 2
As can be seen from Table 1, the high-film-thickness epoxy primers prepared by the preparation method of the invention in examples 1-5 have a limiting film thickness of more than 200 μm, a smooth surface, no shrinkage cavity, excellent flexibility, hardness, water resistance and other properties, and a good film forming effect.
As can be seen from comparison between example 1 and comparative examples 1-2, the epoxy component A is not contained in comparative example 1, the epoxy resin C is not contained in comparative example 2, and the performances of the prepared high-film-thickness epoxy primer are different from those of the high-film-thickness epoxy primer prepared in example 1, because three epoxy resins with different equivalent weights are compounded to form a synergistic enhancement effect among the three epoxy resins, the waterborne epoxy emulsion is endowed with excellent viscosity and is not easy to block, so that the primer formed by the high-film-thickness epoxy primer prepared by the waterborne epoxy emulsion has a smooth surface, and the limit film thickness is improved without cracking.
As can be seen from the example 1 and the comparative example 3, the epoxy resin A in the comparative example 3 is not aminated, but the epoxy resin A in the example 1 is aminated, so that the formed epoxy resin cured product has higher strength and elongation at break, and the surface of the prepared epoxy primer with high film thickness is not easy to crack.
Claims (9)
1. The water-based epoxy emulsion is characterized by comprising the following components in parts by weight: 1-2 parts of epoxy component A, 43-50 parts of epoxy resin B, 6-8 parts of cosolvent B, 4-6 parts of emulsifier, 0.1-0.2 part of dispersant, 35-40 parts of water and 0.2-0.3 part of epoxy resin C;
the epoxy component A comprises the following components in percentage by weight: 62-68% of epoxy resin A, 15-22% of cosolvent A and 14-20% of diethanolamine;
the epoxy resin A is solid epoxy resin, and the epoxy equivalent is 450-1000g/eq;
the epoxy resin B is solid epoxy resin, and the epoxy equivalent is 450-1000g/eq;
the epoxy resin C is liquid epoxy resin, and the epoxy equivalent is 180-190g/eq.
2. The aqueous epoxy emulsion according to claim 1, wherein the cosolvent A is an alcohol ether cosolvent, the alcohol ether cosolvent adopts one or both of butyl cellosolve and propylene glycol methyl ether, and the cosolvent B and the cosolvent A have the same components.
3. The high-film-thickness epoxy primer comprises the water-based epoxy emulsion as recited in claim 1, wherein the high-film-thickness epoxy primer is composed of a component A and a component B, and the mass ratio of the component A to the component B is 6-8:1;
wherein the component A comprises the following components in parts by weight: 35-45 parts of water-based epoxy emulsion, 1-2 parts of propylene glycol methyl ether, 0.1-0.2 part of defoaming agent, 0.4-0.5 part of dispersing agent, 0.1-0.2 part of wetting and leveling agent, 0.5-1 part of anti-flash rust agent, 0.1-0.2 part of montmorillonite clay, 0.3-0.5 part of dipropylene glycol butyl ether, 5-8 parts of anti-rust pigment, 3-5 parts of titanium white, 0.1-0.2 part of carbon black, 20-23 parts of barium sulfate, 24-27 parts of water A and 0.3-0.5 part of thickening agent;
the component B comprises the following components in parts by weight: 45-50 parts of epoxy curing agent, 10-15 parts of propylene glycol monomethyl ether and 45-50 parts of water B.
4. The method for preparing the epoxy primer with high film thickness according to claim 3, comprising the following steps:
a: preparing a water-based epoxy emulsion;
b: weighing the components according to the proportion of the high-film-thickness epoxy primer for later use;
c: adding water A, 40-60% of the content of the defoaming agent, a dispersing agent and propylene glycol methyl ether into a container, uniformly stirring, adding montmorillonite clay, dipropylene glycol butyl ether, an anti-rust pigment, carbon black, titanium white and barium sulfate, uniformly stirring to obtain a mixed slurry, and grinding the mixed slurry to the fineness of less than or equal to 25 mu m to obtain a prophase slurry;
d: c, adding the water-based epoxy emulsion, the dipropylene glycol butyl ether, the early-stage slurry obtained in the step C, the wetting and leveling agent and the residual defoaming agent into another container, uniformly stirring, adding the thickening agent, and uniformly stirring to obtain a component A;
e: and (3) uniformly mixing the epoxy curing agent and the propylene glycol monomethyl ether, adding the water B, and uniformly stirring to obtain the component B.
5. The method for preparing the high film thickness epoxy primer according to claim 4, wherein the step A of preparing the water-based epoxy emulsion comprises the following steps:
a1: weighing the components according to the proportion of the water-based epoxy emulsion for later use;
a2: pouring the epoxy resin A and the cosolvent A into a container, heating until the epoxy resin A is completely melted, adding diethanolamine into the container, carrying out amination, and carrying out amination to obtain an epoxy component A;
a3: and (3) adding the epoxy resin B, the cosolvent B and the emulsifier into another container, heating until the epoxy resin B is completely melted, then sequentially adding the dispersant, 30-40% of the total amount of water, 30-40% of the epoxy component A obtained in the step A2, and the rest water, stirring after adding the components each time, adding the epoxy resin C, stirring in a heating and heat-preserving state, and filtering to obtain the water-based epoxy emulsion.
6. The method for preparing the epoxy primer with high film thickness according to claim 5, wherein the amination is performed after the diethanolamine is added in the step A2 and the reaction is performed for 1.5 to 2.5 hours at 115 to 125 ℃.
7. The method for preparing the epoxy primer with high film thickness according to claim 5, wherein the stirring in the heating and heat preservation state in the step A3 is performed at 85-95 ℃ for 2-4h at a rotating speed of 500-800 r/min.
8. The method for preparing the high-film-thickness epoxy primer according to claim 4, wherein the step C of uniformly stirring to obtain the mixed slurry is to stir at 700-800 r/min for 15-20 min.
9. The method for preparing the high-film-thickness epoxy primer according to claim 4, wherein the water B is added in the step E and stirred uniformly at a speed of 400-500 r/min for 10-20min.
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