CN115806763B - High-pigment-ratio water-based epoxy paint and preparation method and application thereof - Google Patents
High-pigment-ratio water-based epoxy paint and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a high-pigment-ratio water-based epoxy coating which comprises the following components in parts by weight: and (3) a component A: 20 to 35 parts of aqueous epoxy emulsion, 2 to 10 parts of coloring pigment, 4 to 10 parts of antirust pigment, 30 to 50 parts of filler, 0.2 to 0.6 part of dispersing agent, 0.1 to 0.5 part of defoamer, 0.1 to 0.5 part of wetting agent and 0 to 2 parts of thickener; and the component B comprises the following components: 25-50 parts of aqueous epoxy curing agent, 5-10 parts of epoxy-terminated phenyl perfluoropolyether, 0-1 part of flash rust inhibitor, 3-15 parts of film forming auxiliary agent and 0-5 parts of defoaming agent. According to the invention, the epoxy-terminated phenyl perfluoropolyether is added into the component containing the curing agent as the modifier of the curing agent in the aqueous epoxy coating system, so that the compatibility of the curing agent and the aqueous epoxy emulsion matrix and the wettability of pigment and filler are improved, and the high-pigment-ratio aqueous epoxy coating with excellent corrosion resistance can be obtained.
Description
Technical Field
The invention relates to the technical field of water-based anticorrosive paint, in particular to a high-pigment-ratio water-based epoxy paint, and a preparation method and application thereof.
Background
Most of the traditional anticorrosive coatings are solvent-type coatings, which contain a large amount of organic solvents, and the solvents are released in the production and construction processes, so that the solvents are harmful to the health of constructors and pollute the environment. The water paint is an environment-friendly paint which takes water as a solvent, volatilizes water in the use process and is harmless to the environment. The water-based anticorrosive paint has the characteristics of energy conservation, environmental protection and safe use, and becomes a hot spot for competitive research and development of the paint world at home and abroad. At present, the intermediate paint on the market mostly adopts a water-based epoxy cloud iron system, has relatively high price and cost, and has the defects of poor corrosion resistance and poor sagging property.
Along with the continuous progress of society, the requirements of people on water paint are continuously improved, so that the water paint is environment-friendly and nontoxic, and more requirements are provided for the performance of the water paint. If better sagging performance, anti-corrosion performance and adhesion performance are required; meanwhile, in order to achieve better coloring effect, multiple times of painting are often needed, so that the cost is increased, the production efficiency is reduced, and the defects of poor anti-corrosion performance and poor sagging property of a paint film caused by incomplete curing of intermediate paint are easily caused in the multiple times of painting process. The paint frequency can be reduced by increasing the pigment content (namely high pigment ratio) in the water paint, and the paint can have good coloring effect and good covering power even by only one-time painting; however, increasing the pigment base ratio results in a paint film with poorer corrosion resistance.
Therefore, there is a need to develop a high pigment ratio aqueous epoxy coating having excellent corrosion resistance.
Disclosure of Invention
The invention aims to overcome the defect that the pigment ratio and the corrosion resistance of the existing water-based paint cannot be improved at the same time, and develop the high pigment ratio water-based epoxy paint with excellent corrosion resistance. According to the invention, the epoxy-terminated phenyl perfluoropolyether is added into the components containing the curing agent as the modifying agent in the aqueous epoxy coating system, so that the epoxy-terminated phenyl perfluoropolyether forms a long-chain aqueous epoxy curing agent, the benzene ring structure can increase the compatibility with epoxy resin, and the epoxy resin can be more easily dispersed into the coating system for crosslinking and curing, thereby improving the corrosion resistance of a paint film; the long-chain perfluoropolyether structure can increase the strong hydrophilicity of the segments of the curing agent, can greatly reduce the surface tension of the system, and enables the pigment and filler to be easier to wet and disperse, thereby improving the fluidity of the coating and adding more pigment and filler.
The invention further aims at providing a preparation method of the high-pigment-ratio water-based epoxy coating.
It is another object of the present invention to provide the use of the high aspect ratio waterborne epoxy coating in the construction or corrosion protection field.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the high-pigment-ratio water-based epoxy coating comprises the following components in parts by weight:
component A (total 100 parts):
wherein the ratio of the total weight of the coloring pigment, rust inhibitive pigment and filler to the weight of the aqueous epoxy emulsion is >1.5;
component B (total 100 parts):
in general, the addition of inorganic fillers such as pigments and fillers results in a deterioration of the fluidity of the aqueous epoxy system, a decrease in the degree of crosslinking and curing, and further a deterioration of the corrosion resistance of the resulting film. The inventor of the present invention found through research that the addition of epoxy-terminated phenyl perfluoropolyether as a curing agent modifier to a B component containing a curing agent can significantly improve the performance of the coating after film formation.
In the epoxy phenyl perfluoropolyether of the modifier, the epoxy groups can react with the aqueous epoxy curing agent to form a long-chain aqueous epoxy curing agent. 1) The long-chain perfluoropolyether chain segment has strong hydrophilicity, can greatly reduce the surface tension of a system, and enables pigment filler to be more easily wetted and dispersed, so that the fluidity of inorganic pigment filler in a coating matrix can be improved, and more pigment filler can be added; 2) In the epoxy phenyl perfluoropolyether of the modifier, the bond energy of the C-F bond is larger, the stability is strong, the epoxy phenyl perfluoropolyether can not react with various strong oxidants, strong acids and strong bases to be decomposed, and the epoxy phenyl perfluoropolyether is stable in electrolyte, so that the corrosion resistance of the coating can be improved; 3) Meanwhile, the introduction of the terminal benzene ring structure can also increase the compatibility of the epoxy resin and the water-based epoxy curing agent, and can drive the mobility of the water-based epoxy curing agent in the water-based epoxy emulsion matrix, so that the water-based epoxy curing agent is fully crosslinked with the water-based epoxy resin in the water-based epoxy emulsion, and the corrosion resistance of the coating after film formation is further improved.
Preferably, the weight ratio of the aqueous epoxy curing agent to the epoxy phenyl perfluoropolyether is (2.5-10): 1. in the proportion range, the epoxy-terminated phenyl perfluoropolyether can well modify the curing agent so as to improve the coating performance, and the crosslinking density is not influenced by excessive consumption of active hydrogen in the curing agent, so that the effect of the modifier is optimal.
Preferably, the aqueous epoxy emulsion is a nonionic aqueous epoxy emulsion, and the epoxy equivalent is 600-1200 g/mol.
Preferably, the aqueous epoxy curing agent is a self-emulsifying amine curing agent, and the active hydrogen equivalent of the aqueous epoxy curing agent is 100-300 g/mol.
Preferably, in the epoxy phenyl perfluoropolyether, the number average molecular weight of the perfluoropolyether is 500 to 5000. With the increase of the molecular weight of the perfluoropolyether, the viscosity of the perfluoropolyether is increased, after the perfluoropolyether is used for modifying the curing agent, the migration speed of the curing agent in the aqueous epoxy resin matrix is reduced when the components A, B are mixed before the use, the coating is unevenly cured, and the corrosion resistance of the coating is reduced after the coating is formed into a film; when the molecular weight of the perfluoropolyether is low, the chain segment is short, the wettability to pigment and filler is insufficient, and a large amount of pigment and filler tends to agglomerate in the system, so that the corrosion resistance of the coating after film formation is reduced. Therefore, in the above-mentioned suitable molecular weight range, a high pigment ratio aqueous epoxy paint excellent in corrosion resistance can be obtained. The number average molecular weight of the perfluoropolyether is more preferably 1000 to 3000.
In the present invention, conventional pigments, fillers, dispersants, defoamers, wetting agents, thickeners, flash rust inhibitors, and film forming aids may be used in the present invention.
The coloring pigment comprises at least one of iron oxide black, iron oxide red, carbon black and titanium dioxide; the rust inhibitive pigment includes, but is not limited to, at least one of zinc phosphate, zinc molybdate, and aluminum tripolyphosphate; the filler includes, but is not limited to, at least one of talc, precipitated high gloss barium sulfate, mica powder, calcined kaolin, and silica micropowder.
The dispersant includes but is not limited to anionic carboxylate, cationic quaternary amine and nonionic high molecular weight polymer dispersant.
The defoamers include, but are not limited to, silicone based defoamers, ether based defoamers, silicone based defoamers, and mineral oil based defoamers.
The thickener includes, but is not limited to, polyurethane type thickeners, alkali swellable thickeners.
The wetting agents include, but are not limited to, silicone based wetting agents, anionic based wetting agents, nonionic based wetting agents.
The anti-flash rust agent comprises, but is not limited to, traditional hydrochloric acid anti-flash rust agents and organic polymer compound anti-flash rust agents.
The coalescents include, but are not limited to, dodecanol ester, propylene glycol, dipropylene glycol butyl ether, diethylene glycol butyl ether, propylene glycol diacetate.
The invention also provides a preparation method of the high-pigment-ratio water-based epoxy paint, which comprises the following steps:
and (3) preparing a component A:
adding a dispersing agent, a defoaming agent, a coloring pigment, a filler and an antirust pigment into water according to the weight parts, uniformly mixing and dispersing, and grinding to obtain slurry; then uniformly mixing and dispersing the slurry, the aqueous epoxy emulsion, the wetting agent and the thickening agent to obtain the component A;
and (2) preparing a component B:
s1, preparing epoxy-terminated phenyl perfluoropolyether
Uniformly mixing monomers containing epoxy groups and phenyl groups and perfluoropolyether in a solvent, and then completely reacting at 90-120 ℃ to obtain the epoxy-terminated phenyl perfluoropolyether;
s2, uniformly mixing the water-based epoxy curing agent and the epoxy phenyl perfluoropolyether, and reacting at 40-50 ℃ to obtain the modified epoxy curing agent after the reaction is completed; and then uniformly mixing the obtained modified epoxy curing agent, the flash rust inhibitor, the film forming auxiliary agent, the thickening agent and the defoaming agent in water to obtain the component B.
Wherein, in the preparation of the component A, the fineness of the slurry is less than or equal to 50 mu m.
The invention also protects the application of the high-pigment-ratio water-based epoxy paint in the anti-corrosion field, and in particular, the high-pigment-ratio water-based epoxy paint can be coated on the surfaces of petrochemical materials, vehicles such as automobiles, trains, ships and the like, and structures such as bridges, iron towers, doors and windows and the like. Before coating, the component A and the component B are uniformly mixed and then coated on the surface of the substrate for curing. The component A and the component B are prepared according to the following steps of (5-15): 1 by weight.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the epoxy-terminated phenyl perfluoropolyether is added into the component containing the curing agent as the modifier of the curing agent in the aqueous epoxy coating system, so that the compatibility of the curing agent and the aqueous epoxy emulsion matrix and the wettability of pigment and filler are improved, and the high-pigment-ratio aqueous epoxy coating with excellent corrosion resistance can be obtained.
In the water-based epoxy coating system, the pigment base ratio is more than 1.5 and can reach 3.5; the cured film is excellent in corrosion resistance.
Detailed Description
For a better description of the objects, technical solutions and advantages of the present invention, the present invention will be further described with reference to the following specific examples, which are not intended to limit the present invention in any way. Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art. The reagents and materials used in the present invention are commercially available unless otherwise specified.
The following raw materials were used in the examples and comparative examples of the present invention:
aqueous epoxy emulsion:
1#: banco 5550B, epoxy equivalent of 850g/mol, available from co-curing chemistry;
2#: epikote 6520-WH-53A, having an epoxy equivalent of 1040g/mol, available from Guangzhou City fast commercial Co., ltd;
3#:3EE109W, epoxy equivalent 800g/mol, available from Hendel resin;
aqueous epoxy curing agent:
1#: amine curing agent, aradur38-1, with active hydrogen equivalent of 150g/mol, purchased from Guangzhou municipal pick rhyme chemical Co., ltd;
2#: amine curing agent, L-920-50H, active hydrogen equivalent of 200g/mol, purchased from Dongguan three-lacquer chemical raw material Co., ltd;
fluorine-containing polyether:
1#: perfluoropolyether (PFPE), PFPE-500, having an average number average molecular weight of 500, available from hubei Yongku technologies, inc;
2#: perfluoropolyether (PFPE), PFPE-1000, with an average number average molecular weight of 1000, available from hubei Yongku technologies, inc;
3#: perfluoropolyether (PFPE), PFPE-2000, average number average molecular weight 2000, available from hubei Yongkuan technologies, inc;
4#: perfluoropolyether (PFPE), PFPE-3000, average number average molecular weight 3000, available from hubei Yongkuan technologies, inc;
5#: fluoropolyethers, FPE-2000, having an average number average molecular weight of 1000, available from Hubei Yongkuan technologies Co., ltd;
perfluoropolyether end group modifier:
epoxy resin (containing phenyl groups): e-51, available from Guangzhou chemical industry Co., ltd;
epoxy compound: epichlorohydrin, commercially available;
phenyl-containing compounds: bisphenol a, commercially available;
coloring pigment: iron oxide black, commercially available;
rust-preventive pigment: zinc phosphate, commercially available;
and (3) filling: talc, commercially available;
dispersing agent: AFCONA-5010, available from Epfukana;
defoaming agent: MD-20, available from air chemistry;
wetting agent: 270, purchased from digao;
and (3) a thickening agent: WT-105A, purchased from Haiming-off;
flash rust inhibitor: sodium nitrite, commercially available;
film forming auxiliary agent: propylene glycol, commercially available;
defoaming agent: MD-20, available from air chemistry.
Examples 1 to 12 and comparative examples 1 to 3
Providing a series of aqueous epoxy paint, which is prepared by the following steps:
and (3) preparing a component A:
adding a dispersing agent, a defoaming agent, a coloring pigment, a filler and an antirust pigment into water according to the formula shown in tables 2-3, uniformly mixing and dispersing, and grinding to obtain slurry with fineness less than or equal to 50 mu m; then uniformly mixing and dispersing the slurry, the aqueous epoxy emulsion, the wetting agent and the thickening agent to obtain the component A;
and (2) preparing a component B:
s1, preparing epoxy-terminated phenyl perfluoropolyether
Uniformly mixing a perfluoropolyether end group modifier and perfluoropolyether in water according to a molar ratio of 2.05:1, and then reacting at 95 ℃ for about 4 hours to obtain the epoxy phenyl perfluoropolyether (see table 1);
s2, uniformly mixing a water-based epoxy curing agent and epoxy phenyl perfluoropolyether, reacting at 45 ℃ for about 2 hours to obtain a modified epoxy curing agent according to the formula shown in tables 2-3; and then uniformly mixing the obtained modified epoxy curing agent, the flash rust inhibitor, the film forming auxiliary agent, the thickening agent and the defoaming agent in water to obtain the component B.
TABLE 1 epoxy phenyl perfluoropolyether at the end and monomer formulation (mol)
Table 2 formulations (parts by weight) of waterborne epoxy coatings of examples 1-10
Table 3 formulations (parts by weight) of the waterborne epoxy coatings of examples 11 to 12 and comparative examples 1 to 3
Performance testing
The properties of the aqueous epoxy coatings obtained in the above examples and comparative examples were characterized, and the aqueous epoxy coatings obtained in the above examples were applied to the surface of a sandblasted steel sheet for testing (coating thickness of 250 μm), and specific test items and test methods and results were as follows:
1. after uniformly mixing the component A and the component B, testing the viscosity of the water-based epoxy paint by using a viscometer at room temperature (25 ℃);
2. corrosion resistance:
2.1 acid resistance: the test was performed with reference to the method in standard GBT 50393-2017, the foaming time was observed, and the test parameters were: 5wt% H 2 SO 4 The solution is not foamed, rusted, fallen off and cracked in a certain time period;
2.2 alkali resistance: the test was performed with reference to the method in standard GBT 50393-2017, the foaming time was observed, and the test parameters were: a 5wt% NaOH solution, observing how long it can be done without bubbling, rust, falling, cracking;
2.3 brine tolerance: the test was performed with reference to the method in standard GBT 50393-2017, the foaming time was observed, and the test parameters were: 5wt% NaCl solution, observing how long it can be without bubbling, rust, falling off, cracking;
2.4 salt spray resistance: the test was performed with reference to the method in standard GBT 50393-2017, the foaming time was observed, and the test parameters were: neutral salt fog, no bubbling, no rust, no falling and no cracking can be observed in how long;
3. adhesion test: reference to the method in standard GBT 50393-2017.
The test results are shown in Table 4.
Table 4 results of Performance test of waterborne epoxy coatings obtained in examples and comparative examples
From the above results, it can be seen that:
the high pigment ratio water-based epoxy paint prepared by the invention has pigment ratio of more than 1.5 and can reach 3.5; the cured film is excellent in corrosion resistance and adhesion.
The results of examples 1 to 4 show that a high pigment-ratio aqueous epoxy paint excellent in corrosion resistance and adhesion can be obtained within the above-mentioned amount range of the present invention.
The results of examples 1 and 5-6 show that the conventional epoxy emulsion can be used in the invention within the proper range, the change of the epoxy equivalent has little influence on the performance, and the obtained water-based epoxy coating has better comprehensive performance.
The results of examples 1 and 7-9 show that as the molecular weight of the perfluoropolyether in the epoxy-terminated phenyl perfluoropolyether increases, the viscosity of the perfluoropolyether increases, which, after modifying the curing agent, when the A, B components are mixed before use, can lead to a decrease in the migration rate of the curing agent in the aqueous epoxy resin matrix, lead to uneven curing of the coating, and further lead to a decrease in the corrosion resistance of the coating after film formation; when the molecular weight of the perfluoropolyether is low, the chain segment is short, the wettability to pigment and filler is insufficient, and a large amount of pigment and filler tends to agglomerate in the system, so that the corrosion resistance of the coating after film formation is reduced.
The results of example 1 and example 10 show that conventional curing agents can be used in the present invention.
The results of examples 1 and 11-12 show that the weight ratio of the aqueous epoxy curing agent to the epoxy-terminated phenyl perfluoropolyether is in a proper proportion range, and the epoxy-terminated phenyl perfluoropolyether can not only well modify the curing agent so as to improve the coating performance, but also can not excessively consume active hydrogen in the curing agent to influence the crosslinking density, so that the effect of the modifier is optimal.
In comparative example 1, epoxy-terminated phenyl perfluoropolyether is not added, and in comparative example 3, epoxy resin, perfluoropolyether and phenyl-containing compound are physically mixed to serve as a curing agent modifier, and the wettability to pigment and filler is poor, so that the performances of corrosion resistance, adhesive force and the like of the obtained water-based epoxy coating are obviously reduced; in comparative example 2, phenyl is introduced into the middle of a fluorine-containing polyether chain segment, and the epoxy phenyl fluorine-containing polyether modifier is self-crosslinked due to the need of selecting branched chain polyfunctional fluorine-containing polyether, and cannot be used as a modifier of a curing agent, so that the viscosity of the component B is obviously increased, and the component B cannot be mixed with the component A to prepare a coating.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the technical solution of the present invention may be modified or substituted equally without departing from the spirit and scope of the technical solution of the present invention.
Claims (8)
1. The high-pigment-ratio water-based epoxy coating is characterized by comprising the following components in parts by weight:
and a component A, wherein the total weight is 100 parts:
20-35 parts of aqueous epoxy emulsion;
2-10 parts of coloring pigment;
4-10 parts of rust-proof pigment;
30-50 parts of filler;
0.2-0.6 parts of dispersing agent;
0.1-0.5 part of defoaming agent;
0.1-0.5 part of wetting agent;
0-2 parts of a thickening agent;
the balance of water;
wherein the ratio of the total weight of the coloring pigment, rust inhibitive pigment and filler to the weight of the aqueous epoxy emulsion is >1.5;
and the component B comprises 100 parts by weight:
25-50 parts of a water-based epoxy curing agent;
5-10 parts of epoxy-terminated phenyl perfluoropolyether;
0-1 part of flash rust inhibitor;
3-15 parts of film forming auxiliary agent;
0-5 parts of a defoaming agent;
the balance of water;
the weight ratio of the aqueous epoxy curing agent to the epoxy phenyl perfluoropolyether is (2.5-10): 1, a step of; in the epoxy phenyl perfluoropolyether, the number average molecular weight of the perfluoropolyether is 500-5000; the active hydrogen equivalent of the aqueous epoxy curing agent is 100-300 g/mol;
in the preparation process of the component B, the water-based epoxy curing agent and the epoxy phenyl perfluoropolyether are uniformly mixed and then react at 40-50 ℃ to obtain the modified epoxy curing agent after the reaction is completed.
2. The high aspect ratio aqueous epoxy coating of claim 1, wherein the aqueous epoxy emulsion has an epoxy equivalent of 600 to 1200g/mol; the aqueous epoxy curing agent is a self-emulsifying amine curing agent.
3. The high pigment ratio aqueous epoxy coating of claim 1, wherein the number average molecular weight of the perfluoropolyether in the epoxy phenyl perfluoropolyether is 1000 to 3000.
4. The high aspect ratio waterborne epoxy coating of claim 1, comprising at least one of the following features:
1) The dispersing agent comprises at least one of anionic carboxylate, cationic quaternary amine salt and nonionic high molecular weight polymer dispersing agent;
2) The defoaming agent comprises at least one of an organic silicon defoaming agent, an ether defoaming agent and a mineral oil defoaming agent;
3) The coloring pigment comprises at least one of iron oxide black, iron oxide red, carbon black and titanium dioxide;
4) The rust-proof pigment comprises at least one of zinc phosphate, zinc molybdate and aluminum tripolyphosphate;
5) The filler comprises at least one of talcum powder, precipitated highlight barium sulfate, mica powder, calcined kaolin and silicon micropowder;
6) The thickener comprises at least one of polyurethane thickener and alkali swelling thickener;
7) The wetting agent comprises at least one of organic silicon wetting agent, anionic wetting agent and nonionic wetting agent;
8) The anti-flash rust agent comprises at least one of traditional hydrochloric acid anti-flash rust agents and organic polymer compound anti-flash rust agents;
9) The film forming aid comprises at least one of dodecyl alcohol ester, propylene glycol, dipropylene glycol butyl ether, diethylene glycol butyl ether and propylene glycol diacetate.
5. The method for preparing the high-pigment-ratio water-based epoxy paint as claimed in any one of claims 1 to 4, which is characterized by comprising the following steps:
and (3) preparing a component A:
adding a dispersing agent, a defoaming agent, a coloring pigment, a filler and an antirust pigment into water according to the weight parts, uniformly mixing and dispersing, and grinding to obtain slurry; then uniformly mixing and dispersing the slurry, the aqueous epoxy emulsion, the wetting agent and the thickening agent to obtain the component A;
and (2) preparing a component B:
s1, preparing epoxy-terminated phenyl perfluoropolyether
Uniformly mixing monomers containing epoxy groups and phenyl groups and perfluoropolyether in a solvent, and then completely reacting at 90-120 ℃ to obtain the epoxy-terminated phenyl perfluoropolyether;
s2, uniformly mixing the water-based epoxy curing agent and the epoxy phenyl perfluoropolyether, and reacting at 40-50 ℃ to obtain a modified epoxy curing agent after the reaction is completed; and then uniformly mixing the obtained modified epoxy curing agent, the flash rust inhibitor, the film forming auxiliary agent, the thickening agent and the defoaming agent in water to obtain the component B.
6. The process according to claim 5, wherein the fineness of the slurry in the preparation of the A-component is 50 μm or less.
7. The application of the high-pigment-ratio water-based epoxy paint as claimed in any one of claims 1 to 4 in the field of corrosion prevention.
8. The application of claim 7, wherein in the application process, the component a and the component B are uniformly mixed and then coated on the substrate, and the weight ratio of the component a to the component B is (5-15): 1.
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