CN109337487B - Water-based acrylic amino baking paint - Google Patents
Water-based acrylic amino baking paint Download PDFInfo
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- CN109337487B CN109337487B CN201811110658.2A CN201811110658A CN109337487B CN 109337487 B CN109337487 B CN 109337487B CN 201811110658 A CN201811110658 A CN 201811110658A CN 109337487 B CN109337487 B CN 109337487B
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09D133/062—Copolymers with monomers not covered by C09D133/06
- C09D133/066—Copolymers with monomers not covered by C09D133/06 containing -OH groups
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
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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
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1656—Antifouling paints; Underwater paints characterised by the film-forming substance
- C09D5/1662—Synthetic film-forming substance
- C09D5/1668—Vinyl-type polymers
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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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
- C09D5/16—Antifouling paints; Underwater paints
- C09D5/1687—Use of special additives
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- 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
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Abstract
The invention discloses a water-based acrylic amino baking varnish, which comprises the following components in parts by weight: resin-free color paste; a modified aqueous hydroxyacrylic acid dispersion; a water-soluble amino resin; ethylene glycol monobutyl ether; water; an auxiliary agent; defoaming agents; a defoaming agent; an adhesion promoter; the modified aqueous hydroxy acrylic acid dispersoid is fluorine-containing aqueous hydroxy acrylic acid dispersoid which is obtained by adopting dodecafluoroheptyl methacrylate and hydroxy acrylic acid ester monomers to carry out free polymerization, neutralization and emulsification in an organic solvent and solvent removal; the adhesion promoter is epoxy acrylic acid modified carboxylic ester. Through the arrangement, the acrylic acid dispersoid is changed into the fluorine-containing acrylic acid dispersoid by utilizing the methacrylic acid dodecafluoroheptyl ester, so that the water resistance, weather resistance, pollution resistance, low-temperature flexibility and the like of the baking varnish are obviously improved, and meanwhile, the epoxy acrylic acid modified carboxylic ester is used as the adhesion promoter, so that the adhesion strength with the base material is further improved, the mutual compensation is realized, and the performance is more excellent.
Description
Technical Field
The invention relates to the technical field of baking varnish preparation, and particularly relates to water-based acrylic amino baking varnish.
Background
In the present day of rapid industrial development, manufacturers pay attention to how to improve the workpiece yield and also consider how to ensure the excellent coating effect of the workpiece, so that the problem of dip coating is well solved. The dip coating is a coating construction mode which is convenient to operate, high in coating utilization rate and higher in working efficiency, but the traditional oil dip coating has a plurality of adverse factors of high VOC content, high pollution and strong pungent taste, so that the gradual water-based paint is more accepted and pursued by the market, the water-based paint on the market is unprecedented, but the development space is larger, the development is freer, the water-based paint on the market is good and uneven in quality, particularly, the water resistance of the water-based paint in the using process is generally reflected in market investigation, a plurality of poor quality problems are caused, and the further development of the water-based paint in the market is hindered.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the water-based acrylic amino baking varnish which has a good water-resistant effect.
The technical purpose of the invention is realized by the following technical scheme: the water-based acrylic amino baking paint comprises the following components in parts by weight:
20-45 parts of resin-free color paste;
40-60 parts of modified aqueous hydroxy acrylic acid dispersoid;
5-15 parts of water-soluble amino resin;
1-5 parts of ethylene glycol monobutyl ether;
8-15 parts of water;
1-5 parts of an auxiliary agent;
0.2-0.5 part of defoaming agent;
0.2-0.5 part of defoaming agent;
1-5 parts of an adhesion promoter;
the modified aqueous hydroxy acrylic acid dispersoid is fluorine-containing aqueous hydroxy acrylic acid dispersoid which is obtained by adopting dodecafluoroheptyl methacrylate and hydroxy acrylic acid ester monomers to carry out free polymerization, neutralization and emulsification in an organic solvent and removing the solvent; the adhesion promoter is epoxy acrylic acid modified carboxylic ester.
By adopting the technical scheme, the hydroxyl acrylic acid is modified by the dodecafluoroheptyl methacrylate to obtain the fluorine-containing aqueous hydroxyl acrylic acid dispersoid, because fluorine is the element with the largest electronegativity, the electronegativity is the strongest, the polarizability is the lowest, the atomic radius is only larger than that of hydrogen, when a fluorine atom replaces an H atom on a C-H bond, the formed C-F bond is extremely short, and the bond energy is up to 460KJ/mol, a perfluoro group in the fluorine-containing modified aqueous hydroxyl acrylic acid monomer is positioned on a molecular side chain, the perfluoro group is enriched on an interface of the monomer contacting with air and extends into the air in the film forming process, the main chain and internal molecules can be protected because the perfluoro side chain tends to be outward, and meanwhile, the radius of the fluorine atom is larger than that of the hydrogen atom but smaller than that of other elements, so that the C-C main chain can be tightly wrapped, therefore, the fluorine modified aqueous acrylic acid dispersoid has stronger chemical inertness, thereby having excellent waterproof property, water resistance and good film forming property.
Although the surface energy of the polymer is greatly reduced due to the modification effect of fluorine, the water contact angle of a paint film of a baking varnish solution is obviously increased, and the water absorption is reduced, so that the water-based acrylic amino baking varnish has excellent water resistance, weather resistance, stain resistance and low-temperature flexibility, the adhesion between the water-based acrylic baking varnish and a base material is obviously reduced due to the characteristics of increased water contact angle, reduced water absorption and good water resistance brought by fluorine modification, therefore, ethylene glycol monobutyl ether is used as an excellent solvent and a surfactant to play a role in removing dirt and oil stains on the surface of a metal base material and provide a good environment for the contact between the paint film and the base material, and epoxy acrylic modified carboxylic ester is further arranged as an adhesion promoter, and since the epoxy acrylic modified carboxylic ester contains a large number of base material reaction groups, the epoxy acrylic modified carboxylic ester can easily react with hydroxyl groups in a base, the adhesive force of a paint film in a system is greatly improved, the water resistance of the paint film is further improved, and the paint film is matched with the fluorine-containing aqueous hydroxyl acrylic acid dispersion to achieve the combined effect of greatly improving the water resistance.
The invention is further provided with: the weight ratio of the dodecafluoroheptyl methacrylate to the hydroxy acrylate monomers in the preparation of the modified aqueous hydroxy acrylic acid dispersion is 1-10: 100.
Through adopting above-mentioned technical scheme, set for reasonable fluorine content, be favorable to controlling to accomplish certain balance between reinforcing water proofness and the reduction adhesive force, can with the better mutual cooperation of adhesion promoter.
The invention is further provided with: the resin-free color paste is titanium dioxide or water-based resin-free white paste with the concentration of 70 percent.
By adopting the technical scheme, the coating prepared from the titanium dioxide has bright color, high covering power, strong tinting strength, less using amount and multiple varieties, can play a role in protecting the stability of a medium, can enhance the mechanical strength and adhesive force of a paint film, prevent cracks, prevent ultraviolet rays and moisture from permeating and prolong the service life of the paint film.
The invention is further provided with the following components in parts by weight: 25-35 parts of resin-free color paste; 40-50 parts of modified aqueous hydroxy acrylic acid dispersoid; 8-10 parts of water-soluble amino resin; 3-5 parts of ethylene glycol monobutyl ether; 8-10 parts of water; 1-5 parts of an auxiliary agent; 0.2-0.5 part of defoaming agent; 0.2-0.5 part of defoaming agent; 1-5 parts of adhesion promoter.
The invention is further provided that the auxiliary agent comprises the following components in parts by weight: 0.2-0.8 part of wetting and leveling agent; 1-3 parts of a pH regulator; 0.5-1 part of water-based thickening agent; 0.2-0.5 part of film forming agent.
By adopting the technical scheme, the film forming agent can smoothly and uniformly mix all the components to form a film, and the pH regulator is necessary.
The invention is further configured to be prepared by the following steps:
s1, adding an adhesion promoter, a part of water and a part of pH regulator into the modified aqueous hydroxyl acrylic acid dispersoid, and uniformly stirring at a stirring speed of 300-600r/min to obtain a first paint vehicle;
s2, mixing the residual weight of water, the defoaming agent, the resin-free color paste and the film forming agent, and uniformly stirring at a stirring speed of 500-800r/min to obtain a second paint vehicle;
s3, mixing the first paint and the second paint, continuously stirring at the stirring speed of 500-800r/min, and simultaneously adding water-soluble amino resin, ethylene glycol monobutyl ether and a wetting leveling agent to obtain a third paint;
and S4, adding the aqueous thickening agent and the residual weight of pH regulator into the third paint, regulating the viscosity of the third paint to 70-80S, and regulating the pH to 7.0-8.0 to obtain the aqueous acrylic amino baking paint.
The invention is further provided with: stirring in S1 for 10-15 min.
The invention is further provided with: stirring in S2 for 20-25 min.
The invention is further provided with: stirring in S3 for 10-20 min.
The invention is further provided with: the weight ratio of the water added in S1 to the total water is 3-4:10, and the weight ratio of the pH regulator to the total pH regulator is 6-7: 10.
By adopting the technical scheme, the pH regulator is divided into the front part and the rear part and added into the preparation, so that the pH regulator can be more accurately regulated to 7.0-8.0.
In conclusion, the invention has the following beneficial effects: the modified aqueous hydroxyl acrylic acid dispersoid is adopted for fluorine-containing modification, so that the water resistance of the whole paint film is improved, meanwhile, the adhesion promoter is arranged to make up for the defect of insufficient adhesion, and simultaneously, the mutual promotion is carried out to further enhance the water resistance.
Detailed Description
Example 1: a preparation method of a modified water-based hydroxyl acrylic acid dispersoid mainly comprises the following steps:
first step, free polymerization: 60 parts of propylene glycol butyl ether and 41 parts of glycidyl versatate are added into a four-neck flask provided with a stirring device, a spherical condenser tube, a constant-temperature electric heating furnace and a dropping device, nitrogen is introduced, the mixture is stirred and heated to 135 ℃, a mixed solution of 13 parts of acrylic acid, 44 parts of methyl methacrylate, 43 parts of styrene, 18 parts of butyl acrylate, 14 parts of hydroxyethyl methacrylate and 0.8 part of an initiator is started to be added, the temperature is uniformly added and maintained at 135 ℃, the stirring speed is maintained at 360r/min, and the addition is completed within 3.5 h.
Preserving heat for 40min, adding 5.5 parts of acrylic acid, 5 parts of dodecafluoroheptyl methacrylate and 0.15 part of initiator, finishing the addition within 40min, rapidly adding 0.1 part of initiator, preserving heat for 2h, adding 6 parts of hydroxyl-terminated polyester, reacting at 180 ℃ until the acid value is 7.0-8.0, cooling to 75 ℃, adding 6 parts of dimethylethanolamine, and uniformly stirring;
step two, neutralization and emulsification: adjusting the pH value to 7.0, and slowly adding 300 parts of water for emulsification;
step three, solvent removal: filtering and discharging to obtain the milky white fluorine-containing modified water-based hydroxyl acrylic acid dispersoid.
The weight parts are the ratio of parts under the unified weight standard, can be converted into g or kg, and can be determined according to the actual production requirement.
Examples 2 to 6: the components and the corresponding contents of the components are shown in Table 1, wherein the resin-free color paste is 70% of aqueous resin-free white paste, the modified aqueous hydroxy acrylic acid dispersoid is the fluorine-containing modified aqueous hydroxy acrylic acid dispersoid prepared in example 1, the water-soluble amino resin is high-hydroxymethyl amino resin, the defoaming agent is Moussex 941PL, the defoaming agent is Moussex SF 561, the wetting leveling agent is Modarez PW 336, the pH regulator is 10% of DMEA solution, the aqueous thickening agent is RM-8W, and the film forming agent is an aqueous film forming agent.
Among them, the high methylol type amino resin belongs to a polymeric partially alkylated amino resin, mainly containing alkoxymethyl groups and methylol groups, which contains a very small amount of imino groups. Since the alkoxymethyl group is mainly a group of the crosslinking reaction, the crosslinking reaction can be carried out at a higher temperature, the reactivity of the hydroxymethyl group is higher than that of the alkoxymethyl group, and the hydroxymethyl group in the high-hydroxymethyl amino resin has a higher content, so that the curing reaction speed can be increased, the baking temperature can be reduced, and the self-polymerization reaction can be reduced because the high-hydroxymethyl amino resin contains a very small amount of imino groups.
TABLE 1 Components and their corresponding weights (kg) in examples 2-6
Example 7: an aqueous acrylic amino baking varnish, the components of which are as shown in example 2, is prepared by adopting the following steps:
s1, adding an adhesion promoter, 40% of water and 60% of pH regulator into the modified water-based hydroxyl acrylic acid dispersoid, and stirring at a stirring speed of 500r/min for 12min to obtain a first paint vehicle;
s2, mixing the residual weight of water, the defoaming agent, the resin-free color paste and the film forming agent, and stirring for 22min at a stirring speed of 800r/min to obtain a second paint vehicle;
s3, mixing the first paint and the second paint, keeping the stirring speed at 800r/min, stirring for 15min, and simultaneously adding water-soluble amino resin, ethylene glycol monobutyl ether and a wetting leveling agent to obtain a third paint;
and S4, adding the aqueous thickening agent and the residual weight of pH regulator into the third paint, regulating the viscosity of the third paint to 70-80S, and regulating the pH to 7.0 to obtain the aqueous acrylic amino baking paint.
Example 8: an aqueous acrylic amino stoving varnish differing from that of example 7 in that the stirring speed in S1 was 380r/min and the duration was 15 min.
Example 9: an aqueous acrylic amino stoving varnish differing from that of example 7 in that the stirring speed in S2 was 600r/min and the duration was 25 min.
Example 10: an aqueous acrylic amino stoving varnish differing from that of example 7 in that the stirring speed in S3 was 600r/min for a period of 20 min.
Example 11: the difference between the water-based acrylic amino baking paint and the embodiment 2 is that the resin-free color paste adopts titanium dioxide.
Example 12: a method for producing a modified aqueous acrylic dispersion, which is different from example 1 in that 8 parts of dodecafluoroheptyl methacrylate are added.
Comparative examples 1 to 6: an acrylic amino stoving varnish differs from example 2 in that it contains the components and their respective contents shown in table 2.
TABLE 2 comparative examples 1-6 contain the respective components and their respective amounts (kg)
The resin-free color paste is water-based resin-free white paste with the concentration of 70%, the modified water-based hydroxyl acrylic acid dispersoid is the fluorine-containing modified water-based hydroxyl acrylic acid dispersoid prepared in the embodiment 1, the water-soluble amino resin is high-hydroxymethyl amino resin, the defoaming agent is Moussex 941PL, the defoaming agent is Moussex SF 561, the wetting and leveling agent is Modarez PW 336, the pH adjusting agent is 10% DMEA solution, the water-based thickening agent is RM-8W, and the film forming agent is a water-based film forming agent.
Characterization test
The following examples and comparative examples are selected as test components, the finished acrylic amino baking varnish is prepared under the same curing temperature and curing time, the following tests are respectively carried out, the test results are recorded in table 3, wherein the adhesion test adopts a cross-cut method, and the water resistance is 36h test class.
TABLE 3 characterisation of the experimental data
| Components | Hardness of pencil | Adhesion force | Water resistance | Boiling water resistance | Gloss/% | Alkali resistance |
| Example 2 | 4H | Level 0 | No abnormality | No abnormality | 46 | No abnormality |
| Example 6 | 5H | Level 0 | No abnormality | No abnormality | 44 | No abnormality |
| Example 8 | 4H | Level 0 | No abnormality | No abnormality | 45 | No abnormality |
| Example 12 | 4H | Level 0 | No abnormality | No abnormality | 46 | No abnormality |
| Comparative example 1 | 3H | Level 1 | High foaming | High foaming | 42 | Little foaming |
| Comparative example 2 | 3H | Level 1 | High foaming | High foaming | 41 | Little foaming |
| Comparative example 3 | 3H | Level 0 | High foaming | High foaming | 42 | No abnormality |
| Comparative example 4 | 3H | Stage 2 | Little foaming | High foaming | 38 | Little foaming |
| Comparative example 5 | 2H | Stage 2 | Little foaming | High foaming | 39 | Little foaming |
| Comparative example 6 | 2H | Stage 2 | Little foaming | High foaming | 39 | Little foaming |
Claims (8)
1. The water-based acrylic amino baking varnish is characterized by comprising the following components in parts by weight:
25-35 parts of resin-free color paste;
40-50 parts of modified aqueous hydroxy acrylic acid dispersoid;
8-10 parts of water-soluble amino resin;
3-5 parts of ethylene glycol monobutyl ether;
8-10 parts of water;
1-5 parts of an auxiliary agent;
0.2-0.5 part of defoaming agent;
0.2-0.5 part of defoaming agent;
1-5 parts of an adhesion promoter;
the modified aqueous hydroxy acrylic acid dispersoid is fluorine-containing aqueous hydroxy acrylic acid dispersoid which is obtained by adopting dodecafluoroheptyl methacrylate and hydroxy acrylic acid ester monomers to carry out free polymerization, neutralization and emulsification in an organic solvent and removing the solvent; the adhesion promoter is epoxy acrylic acid modified carboxylate;
the weight ratio of the dodecafluoroheptyl methacrylate to the hydroxy acrylate monomers in the preparation of the modified aqueous hydroxy acrylic acid dispersion is 1-10: 100.
2. The aqueous acrylic amino baking varnish according to claim 1, wherein: the resin-free color paste is titanium dioxide or water-based resin-free white paste with the concentration of 70 percent.
3. The water-based acrylic amino baking varnish as claimed in claim 2, wherein the auxiliary comprises the following components in parts by weight:
0.2-0.8 part of wetting and leveling agent;
1-3 parts of a pH regulator;
0.5-1 part of water-based thickening agent;
0.2-0.5 part of film forming agent.
4. The water-based acrylic amino baking varnish according to claim 3, wherein the baking varnish is prepared by the following steps:
s1, adding an adhesion promoter, a part of water and a part of pH regulator into the modified aqueous hydroxyl acrylic acid dispersoid, and uniformly stirring at a stirring speed of 300-600r/min to obtain a first paint vehicle;
s2, mixing the residual weight of water, the defoaming agent, the resin-free color paste and the film forming agent, and uniformly stirring at a stirring speed of 500-800r/min to obtain a second paint vehicle;
s3, mixing the first paint and the second paint, continuously stirring at the stirring speed of 500-800r/min, and simultaneously adding water-soluble amino resin, ethylene glycol monobutyl ether and a wetting leveling agent to obtain a third paint;
and S4, adding the aqueous thickening agent and the residual weight of pH regulator into the third paint, regulating the viscosity of the third paint to 70-80S, and regulating the pH to 7.0-8.0 to obtain the aqueous acrylic amino baking paint.
5. The aqueous acrylic amino baking varnish according to claim 4, wherein: stirring in S1 for 10-15 min.
6. The aqueous acrylic amino baking varnish according to claim 5, wherein: stirring in S2 for 20-25 min.
7. The aqueous acrylic amino baking varnish according to claim 6, wherein: stirring in S3 for 10-20 min.
8. The aqueous acrylic amino baking varnish according to claim 7, wherein: the weight ratio of the water added in S1 to the total water is 3-4:10, and the weight ratio of the pH regulator to the total pH regulator is 6-7: 10.
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| CN110982371B (en) * | 2019-12-18 | 2021-05-14 | 万华化学集团股份有限公司 | Environment-friendly water-based high-gloss high-fullness high-temperature baking varnish |
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| CN111393622A (en) * | 2020-04-29 | 2020-07-10 | 广东邦弗特新材料有限公司 | Saturated polyester resin modified by hydroxyl acrylic fluorine-containing resin and preparation method thereof |
| CN111499851A (en) * | 2020-04-29 | 2020-08-07 | 广东邦弗特新材料有限公司 | Carboxyl acrylic fluorine-containing resin modified saturated polyester resin and preparation method thereof |
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| CN107936730A (en) * | 2017-12-11 | 2018-04-20 | 湖南太子化工涂料有限公司 | A kind of water-based amino-stoving varnish and preparation method thereof |
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