CN111117413B - Single-component water-based epoxy anticorrosive primer and preparation method thereof - Google Patents
Single-component water-based epoxy anticorrosive primer and preparation method thereof Download PDFInfo
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- CN111117413B CN111117413B CN201911361407.6A CN201911361407A CN111117413B CN 111117413 B CN111117413 B CN 111117413B CN 201911361407 A CN201911361407 A CN 201911361407A CN 111117413 B CN111117413 B CN 111117413B
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- 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
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
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- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
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- 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
- C09D5/082—Anti-corrosive paints characterised by the anti-corrosive pigment
- C09D5/084—Inorganic compounds
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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- C08G2150/00—Compositions for coatings
- C08G2150/90—Compositions for anticorrosive coatings
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
Abstract
The invention discloses a single-component aqueous epoxy anticorrosive primer and a preparation method thereof, wherein a main resin emulsion is synthesized by a polyethylene glycol nonionic flexible chain segment through a self-emulsifying method, and simultaneously, an acrylic ester monomer with low price is used for toughening, grafting and modifying the epoxy emulsion, so that an additional curing agent is not needed for curing, the primer has good water resistance and anticorrosive performance, high drying speed, stability and safety, and good matching property with pigments and fillers, solves the problems of brittleness and weather resistance of epoxy resin, and enlarges the application range.
Description
Technical Field
The invention belongs to the technical field of water-based paint, and particularly relates to preparation of a single-component water-based epoxy anticorrosive primer.
Background
In the production and preparation processes of the traditional solvent-based paint, a large amount of toxic and harmful volatile organic compounds (VOC for short) are released, so that the natural environment and the human health are greatly harmed. With the improvement of environmental protection consciousness and the improvement of national laws and regulations, green pollution-free water-based coatings gradually become the development direction of the coating industry. Compared with the traditional solvent-based coating, the water-based coating basically cannot pollute the ecological environment, has advantages in the aspect of environmental protection, and has very wide development prospects in the aspects of household woodware, building internal and external walls, automobile industry and the like.
In recent years, some companies and research units at home and abroad begin to research and develop water-based epoxy emulsion, water-based epoxy curing agent and two-component water-based epoxy resin coating. For example, waterborne epoxy resins and curing agents of Zhejiang Anbang New Material development Co., Ltd, Marine chemical research institute, Hunsmei, Zhanxin, etc. are successively used in steel structure anticorrosion coating engineering. The price of the domestic water-based epoxy emulsion and the water-based epoxy curing agent is obviously lower than that of foreign products, but the products have certain gaps in storage stability and product performance compared with products of foreign major companies.
In addition, most of the water-based epoxy resins on the market are ionic, are easy to flash and sensitive to pH value, limit the use of pigments and fillers, have the problems of large coating brittleness, impact resistance, poor weather resistance and the like in a single water-based epoxy resin,
in addition, most of the anticorrosive coatings on the market are double-component packages, and the anticorrosive coatings are uniformly mixed according to the proportion of one end and then used, so that the construction is limited to a certain extent, and the coating waste can be caused, so that the development of single-component anticorrosive coatings is of practical significance. The existing single-component water-based primer has the problems of poor stability, poor adhesion, bleeding and the like, and needs to be improved urgently.
Disclosure of Invention
In order to solve the problems, the invention provides the single-component water-based epoxy anticorrosive primer and the preparation method thereof, which have the advantages of good water resistance and anticorrosive performance, high drying speed, stability and safety. The specific technical scheme is as follows:
the single-component water-based epoxy anti-corrosion primer comprises the following raw materials in parts by weight:
40-60% of waterborne polyurethane epoxy acrylate emulsion,
1.5 to 2 percent of dispersant,
0.5 to 2 percent of defoaming agent,
0.1-0.5% of substrate wetting agent,
8 to 15 percent of antirust pigment,
0.5 to 3 percent of anti-flash embroidery agent,
1 to 5 percent of thickening agent,
8 to 15 percent of filler,
the balance of deionized water.
Specifically, the anti-rust pigment comprises any one of iron oxide red, iron oxide yellow, mica iron oxide, mica powder, zinc phosphate and glass scales;
specifically, the filler comprises any one of talcum powder, mica powder, natural barite powder, calcite powder and light calcium carbonate;
specifically, the defoaming agent comprises any one of BYK-023, BYK025, BYK033, BYK-AT203 or TEGO Airex 931;
specifically, the dispersing agent comprises any one of BYK-151, BYK-190, TEGO Dispers 715W or TEGO Dispers 752W;
specifically, the substrate wetting agent comprises any one of BYK-301, TEGO Wet 245, TEGO Wet 250 or TEGO Wet 500;
specifically, the thickening agent comprises any one of RM-8W or TEGO ViscoPlus 3060;
specifically, the anti-flash embroidery agent comprises any one of R-760F, R-765 and Raybo 60.
The single-component water-based epoxy anticorrosive primer is synthesized by the following steps:
1) adding a dispersant into water according to a certain proportion, and dispersing for 10min at a low speed;
2) adding the aqueous polyurethane epoxy acrylate emulsion, and dispersing at medium speed for 30 min;
3) adding an anti-flash embroidery agent, an anti-rust pigment and a filler, and dispersing at a medium speed for 30 min;
4) adding the defoaming agent, the substrate wetting agent and the thickening agent, stirring for several minutes for defoaming, stirring at medium and low speed, and fully and uniformly mixing to obtain the coating.
Specifically, the water-based polyurethane epoxy acrylate emulsion comprises the following raw materials in parts by weight:
30 to 40 percent of epoxy resin,
10 to 15 percent of diisocyanate,
15 to 25 percent of polyether glycol,
20-30% of acrylic ester,
3 to 8 percent of initiator
0.5 to 1 percent of PH regulator,
the balance of deionized water.
Specifically, the polyether polyol comprises any one of polyethylene glycol 1000, polyethylene glycol 2000, polyethylene glycol 4000 and polyethylene glycol 6000;
specifically, the diisocyanate comprises any one of liquefied MDI, IPDI, TDI and HDI;
specifically, the epoxy resin comprises any one of bisphenol A type epoxy resin E-51, E-44 and E-20;
specifically, the acrylate monomer comprises any one of methyl (meth) acrylate, styrene, butyl (meth) acrylate, hydroxyethyl (meth) acrylate, hydroxypropyl acrylate and isobornyl (meth) acrylate;
specifically, the initiator comprises any one of BPO, AIBN, ammonium persulfate and potassium persulfate;
specifically, the pH regulator comprises sodium carbonate or sodium bicarbonate.
The waterborne polyurethane epoxy acrylate emulsion comprises the following synthetic steps:
1) putting polyether polyol into a reaction kettle in proportion, dehydrating for 2-3 h at 110 ℃, and checking that the water content is less than or equal to 0.5%;
2) cooling to 60 ℃, adding diisocyanate, stirring, heating to 75 +/-2 ℃, keeping the temperature constant for 2-3 h, measuring the-NCO content by adopting a di-n-butylamine method, cooling to below 60 ℃, defoaming in vacuum for 30min, and discharging to obtain a polyurethane prepolymer;
3) reacting epoxy resin in a certain proportion with the polyurethane prepolymer obtained in the step 2) at 120 ℃ for 2h, and preparing epoxy resin modified polyurethane by condensation of-NCO and-OH in the epoxy resin;
4) adding a pH regulator, an acrylate mixed monomer dissolved with epoxy resin modified polyurethane and deionized water, and stirring at a high speed for pre-emulsification to prepare a pre-emulsion;
5) adding water, stirring and heating to 80 ℃, adding 1/4 the pre-emulsion and part of the initiator prepared in the step 4), stirring until the system has obvious blue light, heating to 85 ℃, starting to uniformly dropwise add the rest pre-emulsion and the rest initiator solution, finishing dropwise adding after 3.5h, keeping the temperature and reacting for 1h, cooling to 40 ℃, and filtering and discharging to obtain the waterborne polyurethane epoxy acrylate emulsion.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides the single-component water-based epoxy anti-corrosion primer and the preparation method thereof, the main resin emulsion is synthesized by adopting a polyethylene glycol nonionic flexible chain segment through a self-emulsifying method, and meanwhile, the epoxy emulsion is toughened, grafted and modified by using the acrylate monomer with low price, so that the paint does not need an additional curing agent to participate in curing, has good water resistance and anti-corrosion performance, high drying speed, stability and safety, and good matching property with pigments and fillers, solves the problems of brittleness and weather resistance of epoxy resin, and enlarges the application range.
Drawings
FIG. 1 is a synthesis route diagram of waterborne polyurethane epoxy acrylate
Detailed Description
For a better understanding of the present invention, the following further illustrates the present invention with reference to specific examples and drawings, but the present invention is not limited to the following examples.
Example 1
The single-component water-based epoxy anti-corrosion primer comprises the following raw materials in parts by weight:
40-60% of waterborne polyurethane epoxy acrylate emulsion, BYK-1511.5% of dispersant, BYK 0251% of defoaming agent, TEGO Wet 2500.2% of substrate wetting agent, 15% of rust-proof pigment iron oxide yellow, R-760F 2% of anti-flash embroidery agent, RM-8W 1% of thickening agent, 9% of filler light calcium carbonate and the balance of deionized water.
The aqueous polyurethane epoxy acrylate emulsion comprises the following raw materials in parts by weight:
bisphenol A type epoxy resin E-4435%, diisocyanate liquefied MDI 15%, polyethylene glycol 200018%, styrene 22%, ammonium persulfate 7%, sodium carbonate 0.5%, and the balance of deionized water.
Example 2
The single-component water-based epoxy anti-corrosion primer comprises the following raw materials in parts by weight:
60% of waterborne polyurethane epoxy acrylate emulsion, 1.7% of dispersant TEGO Dispers 715W, 1.7% of defoamer BYK-0230.5%, 2450.5% of substrate wetting agent TEGO Wet, 13% of mica powder, 600.5% of anti-flash embroidery agent Raybo, 3.4% of thickener RM-8W, 15% of filler calcite powder and the balance deionized water.
The aqueous polyurethane epoxy acrylate emulsion comprises the following raw materials in parts by weight:
bisphenol A type epoxy resin E-2030%, diisocyanate liquefied HDI 11%, polyethylene glycol 100025%, hydroxypropyl acrylate 20%, BPO 3%, sodium carbonate 0.8%, and the balance of deionized water.
Example 3
The single-component water-based epoxy anti-corrosion primer comprises the following raw materials in parts by weight:
40% of waterborne polyurethane epoxy acrylate emulsion, BYK-1901.6% of dispersant, 11.3% of defoamer TEGO Airex9311, 0.1% of substrate wetting agent BYK-3010.1%, 12% of glass flake, 12% of anti-flash embroidery agent Raybo 603%, thickener TEGO ViscoPlus 30601.9%, 8% of filler talcum powder and the balance of deionized water.
The aqueous polyurethane epoxy acrylate emulsion comprises the following raw materials in parts by weight:
bisphenol A epoxy resin E-5132%, diisocyanate liquefied IPDI 10%, polyethylene glycol 600021%, hydroxypropyl acrylate 28%, potassium persulfate 4%, sodium bicarbonate 1%, and the balance of deionized water.
Example 4
The single-component water-based epoxy anti-corrosion primer comprises the following raw materials in parts by weight:
46% of waterborne polyurethane epoxy acrylate emulsion, 752W 2% of dispersant TEGO Dispers, 0332% of defoaming agent BYK, 5000.2% of substrate wetting agent TEGO Wet, 8% of mica iron oxide, R-7651.6% of anti-flash embroidery agent, 30605% of thickener TEGO Visco plus, 10% of filler natural barite powder and the balance of deionized water.
The aqueous polyurethane epoxy acrylate emulsion comprises the following raw materials in parts by weight:
bisphenol A type epoxy resin E-5140%, diisocyanate liquefied TDI 13%, polyethylene glycol 400015%, methyl (meth) acrylate 30%, AIBN 8%, sodium bicarbonate 1%, and the balance of deionized water.
The following preparation methods were adopted in all of the above examples 1 to 4:
synthesis of aqueous polyurethane epoxy acrylate emulsion
Putting polyether polyol into a reaction kettle according to a proportion, dehydrating for 2-3 h at 110 ℃, and detecting that the water content is less than or equal to 0.5%.
Cooling to 60 ℃, adding diisocyanate, stirring, heating to 75 +/-2 ℃, keeping the temperature constant for 2-3 h, measuring the-NCO content by adopting a di-n-butylamine method, cooling to below 60 ℃, defoaming in vacuum for 30min, and discharging to obtain the polyurethane prepolymer.
Reacting epoxy resin and polyurethane prepolymer in a certain proportion at 120 ℃ for 2h, and preparing epoxy resin modified polyurethane by condensation of-NCO and-OH in the epoxy resin.
A pH regulator, an acrylate mixed monomer dissolved with polyurethane modified epoxy resin and deionized water are added into a three-neck flask provided with an electric stirrer and a constant pressure dropping funnel, and pre-emulsification is carried out by high-speed stirring to obtain pre-emulsion.
Adding water into a four-neck flask provided with an electric stirrer, a reflux condenser pipe and a constant-pressure dropping funnel, stirring and heating to 80 ℃, adding 1/4 pre-emulsion and part of initiator, stirring until obvious blue light appears in the system, heating to 85 ℃, starting to uniformly dropwise add the residual pre-emulsion and the residual initiator solution, completing dripping within 3.5 hours, carrying out heat preservation reaction for 1 hour, cooling to 40 ℃, and then filtering and discharging to obtain the waterborne polyurethane epoxy acrylate emulsion.
Two, synthesizing single-component water-based epoxy anti-corrosion primer
Adding a given amount of dispersant into water according to the formula, and dispersing for 10 minutes at a low speed; adding a specified amount of polyurethane epoxy acrylate emulsion, and dispersing at medium speed for about 30 min; adding an anti-flash embroidery agent, an anti-rust pigment and a filler, and dispersing at medium speed for about 30 min; adding the defoaming agent, the substrate wetting agent and the thickening agent, stirring for several minutes to defoam, stirring at a medium-low speed, and fully and uniformly mixing to obtain the coating.
And (3) detecting the drying time, the adhesive force, the impact strength and the hardness of the coating film, and detecting the water resistance and the salt spray resistance of the coating film.
The drying time is GB/T1728-89, the adhesion is GB/T9286-2008, the impact strength is GB/T1732, the hardness is GB/T6739-2006, the water resistance is GB/T1733-1993, the salt spray resistance is GB/T1771, and the test results are as follows:
TABLE 1 Performance index of Single-component waterborne epoxy anticorrosion primer for examples 1-4
| Item | Example 1 | Example 2 | Example 3 | Example 4 |
| Surface drying time/min | 10 | 12 | 12 | 10 |
| Actual drying time/h | 6 | 10 | 10 | 8 |
| Adhesion/grade | 0 | 0 | 1 | 1 |
| Impact strength/cm | ≥50 | ≥50 | ≥50 | ≥50 |
| hardness/H | 2H | 2H | 1H | 1H |
| Water resistance/h | 720h | 600h | 600h | 720h |
| Salt spray resistance/h | 1440h | 1200h | 1320h | 1440h |
As can be seen from the results in Table 1, the single-component waterborne epoxy anticorrosive primer of the invention has various indexes meeting the market requirements, wherein the water resistance and the salt spray resistance have obvious effects compared with similar products.
Claims (4)
1. A single-component waterborne epoxy anticorrosive primer is characterized in that: the raw materials comprise the following components in parts by weight:
40-60% of waterborne polyurethane epoxy acrylate emulsion,
1.5 to 2 percent of dispersant,
0.5 to 2 percent of defoaming agent,
0.1-0.5% of substrate wetting agent,
8 to 15 percent of antirust pigment,
0.5 to 3 percent of anti-flash embroidery agent,
1 to 5 percent of thickening agent,
8 to 15 percent of filler,
the balance of deionized water;
the waterborne polyurethane epoxy acrylate emulsion comprises the following synthetic raw materials in parts by weight:
30 to 40 percent of epoxy resin,
10 to 15 percent of diisocyanate,
15 to 25 percent of polyether glycol,
20-30% of acrylic ester,
3 to 8 percent of initiator
0.5 to 1 percent of PH regulator,
the balance of deionized water;
the acrylate monomer comprises any one of methyl (meth) acrylate, styrene, butyl (meth) acrylate, hydroxyethyl (meth) acrylate, hydroxypropyl acrylate and isobornyl (meth) acrylate;
the synthesis steps of the waterborne polyurethane epoxy acrylate emulsion are as follows:
1) putting polyether polyol into a reaction kettle in proportion, dehydrating for 2-3 h at 110 ℃, and checking that the water content is less than or equal to 0.5%;
2) cooling to 60 ℃, adding diisocyanate, stirring, heating to 75 +/-2 ℃, keeping the temperature constant for 2-3 h, measuring the-NCO content by adopting a di-n-butylamine method, cooling to below 60 ℃, defoaming in vacuum for 30min, and discharging to obtain a polyurethane prepolymer;
3) reacting epoxy resin with the polyurethane prepolymer obtained in the step 2) for 2 hours at 120 ℃, and preparing epoxy resin modified polyurethane by condensation of-NCO and-OH in the epoxy resin;
4) adding a pH regulator, an acrylate mixed monomer dissolved with epoxy resin modified polyurethane and deionized water, and stirring at a high speed for pre-emulsification to prepare a pre-emulsion;
5) adding water, stirring and heating to 80 ℃, adding 1/4 the pre-emulsion and part of the initiator prepared in the step 4), stirring until the system has obvious blue light, heating to 85 ℃, starting to uniformly dropwise add the rest pre-emulsion and the rest initiator solution, finishing dropwise adding after 3.5h, keeping the temperature and reacting for 1h, cooling to 40 ℃, and filtering and discharging to obtain the waterborne polyurethane epoxy acrylate emulsion.
2. The one-component waterborne epoxy corrosion resistant primer according to claim 1, wherein:
the anti-rust pigment comprises any one of iron oxide red, iron oxide yellow, mica iron oxide, mica powder, zinc phosphate and glass flakes;
the filler comprises any one of talcum powder, mica powder, natural barite powder, calcite powder and light calcium carbonate;
the defoaming agent comprises any one of BYK-023, BYK025, BYK033, BYK-AT203 or TEGO Airex 931;
the dispersing agent comprises any one of BYK-151, BYK-190, TEGO Dispers 715W or TEGO Dispers 752W;
the substrate wetting agent comprises any one of BYK-301, TEGO Wet 245, TEGO Wet 250 or TEGO Wet 500;
the thickening agent comprises any one of RM-8W or TEGO Visco plus 3060;
the anti-flash embroidery agent comprises any one of R-760F, R-765 and Raybo 60.
3. The method for preparing the one-component waterborne epoxy anticorrosive primer according to claim 1, wherein: the single-component water-based epoxy anticorrosive primer is synthesized by the following steps:
1) adding a dispersant into water according to a certain proportion, and dispersing for 10min at a low speed;
2) adding the aqueous polyurethane epoxy acrylate emulsion, and dispersing at medium speed for 30 min;
3) adding an anti-flash embroidery agent, an anti-rust pigment and a filler, and dispersing at a medium speed for 30 min;
4) adding the defoaming agent, the substrate wetting agent and the thickening agent, stirring for several minutes for defoaming, stirring at a medium and low speed, and fully and uniformly mixing to obtain the coating.
4. The one-component waterborne epoxy corrosion resistant primer according to claim 1, wherein:
the polyether polyol comprises any one of polyethylene glycol 1000, polyethylene glycol 2000, polyethylene glycol 4000 and polyethylene glycol 6000;
the diisocyanate comprises any one of liquefied MDI, IPDI, TDI and HDI;
the epoxy resin comprises any one of bisphenol A type epoxy resin E-51, E-44 and E-20;
the initiator comprises any one of BPO, AIBN, ammonium persulfate and potassium persulfate;
the pH regulator comprises sodium carbonate or sodium bicarbonate.
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| CN113307918B (en) * | 2021-06-07 | 2022-04-15 | 东莞长联新材料科技股份有限公司 | Vegetable oil-based polyacrylate nonionic emulsion and preparation method and application thereof |
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