CN108070318B - Preparation method and application of self-repairing water-based automobile coating - Google Patents
Preparation method and application of self-repairing water-based automobile coating Download PDFInfo
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
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Abstract
The invention relates to a preparation method and application of a self-repairing water-based automobile coating, belonging to a water-based automobile coating series. It discloses a preparation method of silicon dioxide nanometer modified polyurethane aqueous dispersion. The invention fully combines the special physical and chemical properties of the nano material and the advantages of polyurethanes, develops and develops the waterborne automobile coating with the self-repairing function, ensures that the coating on the surface of the automobile body is slightly damaged, particularly the inner part of the automobile body is not easily detected, realizes the self-repairing of the damaged part of the coating by self under the condition of not using an additional repairing material, and has great value. Meanwhile, the nano particles interact with the framework material to form a paint film which has high gloss, good fullness, excellent mechanical property, greatly improved comprehensive performance, environmental protection, energy conservation, strong operability, convenient popularization and application and wide market prospect.
Description
Technical Field
The invention relates to a preparation method and application of a self-repairing water-based automobile coating, in particular to a preparation method of a silicon dioxide nano-modified polyurethane aqueous dispersion.
Background
With the development of industrial economy and urbanization, the automobile output and sales volume in China is continuously connected with cicada for seven years and is the first world of the largest automobile output and sales country. The rapid development of the automotive industry has a significant pull on the automotive coatings market, making automotive coatings the fastest developing coating variety and the most performance demanding coating variety, and therefore automotive coatings often represent the highest level of development of the contemporary coating industry.
The surface coating for automobiles plays a main role in decoration and protection in the whole coating, and the paint film is required to have plump and smooth appearance, no flaws, sufficient hardness, stone chip resistance, chemical resistance, stain resistance, corrosion resistance and the like. However, no matter how good the automobile coating quality is, in the using process, the coating inevitably generates micro cracks and local damage due to the interference of external factors, such as invasion of slurry, splash stones and mechanical rubbing, damage of adhered objects, tree and tree scraping, scratch and bruise of hard devices and the like, the surface cannot be seen abnormally, but the mechanical strength of the coating is reduced, the integrity is seriously damaged, and due to the limitation of manual repair, the damaged parts cannot be repaired in time, so that the performance of the coating is reduced, the high decoration and luster of the surface are damaged, the service life of the coating is greatly shortened, and the disaster effect is sometimes brought. Therefore, the automobile coating with the self-repairing function is developed, so that the damage to the coating on the surface of an automobile body, especially the damage in the automobile body, which cannot be detected, can be sensed, the self-repairing of the damaged part of the coating can be realized by depending on the performance of the material without using an additional repairing material, and the automobile coating has great value and application prospect.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a preparation method and application of a self-repairing water-based automobile coating, which can realize self-repairing of a damaged part of the coating by means of the performance of the material under the condition that the coating on the surface of an automobile body is slightly damaged without using an additional repairing material, and has great value and application prospect. Meanwhile, the formed paint film is plump and high in gloss, has excellent mechanical property, weather resistance and stability, is water-based and environment-friendly, realizes energy conservation and emission reduction, and is convenient to popularize and apply.
The invention provides a preparation method of a silicon dioxide nanometer modified polyurethane aqueous dispersion, which comprises the following steps:
adding 60-80 parts by weight of polyol (polyethylene glycol, polypropylene glycol or polycarbonate diol, polybutylene adipate diol), 5-10 parts by weight of N-methylpyrrolidone and 0.1-0.5 part by weight of nano silicon dioxide into a reaction kettle provided with a stirring paddle, a thermometer and a condenser, heating to 80 ℃ under the protection of nitrogen, keeping a high-speed dispersion state for 0.5h, adding 3-5 parts by weight of dimethylolbutyric acid, cooling to 65 ℃, adding 0.02-0.05 part by weight of organic tin catalyst (dibutyltin dilaurate, stannous octoate) and 15-25 parts by weight of polyisocyanate (isophorone diisocyanate or diphenylmethane diisocyanate or hexamethylene diisocyanate), keeping the temperature at 80 ℃, continuously reacting for 3-4h, cooling to 55 ℃, adding 2-4 parts by weight of neutralizer (ammonia water or triethylamine or dimethylethanolamine) for neutralization, reacting for 25min until the pH value is 8-9 to obtain the nano modified polyurethane aqueous dispersion prepolymer.
Keeping the prepolymer at 70 ℃, slowly adding the prepolymer into deionized water at 25 ℃ under strong stirring, finally adding a proper amount of ethylenediamine, reacting for 2 hours, and discharging to obtain the silicon dioxide nano-modified polyurethane aqueous dispersion.
According to the construction special requirements of the current automobile surface water-based coating, non-toxic and pollution-free inorganic non-metal nano silicon dioxide is introduced, the nano silicon dioxide has a three-dimensional silica structure, the surface shows stronger activity, hydrogen bond acting force is gathered, nano modified polyurethane aqueous dispersion for automobiles is prepared, and is compounded with water-based acrylic dispersion, and is cross-linked and cured to form a film through hydrophilic modified polyisocyanate, a polyurethane network structure with high cross-linking density is formed, the main chain of a hard and flexible paint film is deformed but not broken under the external scraping action, the hydrogen bond is opened, the main chain is restored after the external force is eliminated, and is recombined again, some scratches can be found from the appearance, and the main chain is stretched under the stress action through external input energy (such as sunshine), the hydrogen bonds also return to their original position and the scratch is reduced or eliminated. In addition, the nano particles are dispersed in the polymer framework and interact with the framework material, which is favorable for improving the toughness and mechanical property of the coating. Such as improving the wear resistance, scratch resistance, hardness, strength and the like of the coating, and simultaneously greatly improving the appearance of the paint film, such as luster, leveling property and the like. The high-performance water-based automobile coating new material with the self-repairing function, prepared by the invention, fills the blank of the domestic water-based automobile coating, and the silicon dioxide nano-modified self-repairing water-based automobile coating is firstly developed, has the advantages of no toxicity, difficult combustion, environmental protection and energy conservation, and has great significance for maintaining the mechanical strength and the decorative effect of the coating, eliminating hidden dangers, prolonging the service life and promoting the water-based development of the domestic original factory repairing coating.
In another application scheme, the invention provides a preparation method of a self-repairing water-based automobile coating, which comprises the following steps:
adopting a resin-free milling system, selecting water-based pigment, deionized water and functional water-based auxiliary agent, uniformly mixing, grinding in a water-based sand mill, adding the nano modified polyurethane water dispersion, the water-based acrylic acid dispersion and the water-based auxiliary agent according to a proper proportion under a dispersion condition, and uniformly stirring to obtain the self-repairing water-based automobile coating product.
The self-repairing water-based automobile coating product is prepared by selectively researching various raw materials and additives, and the basic formula comprises the following components in addition:
the raw materials are added in sequence, and after the raw materials are dispersed and milled to be qualified, the self-repairing water-based paint for the automobile, namely the component A, is obtained. And the modified polyisocyanate is uniformly mixed with hydrophilic modified polyisocyanate serving as a component B according to the proportion of A: B and deionized water being 4:1:0.5-1.5 to obtain a coating product capable of being applied and sprayed.
The hydrophilic modified polyisocyanate of the invention is selected from one or two of modified HDI (Bayhydur 304 of Bayer) or modified IPDI (Bayhydur 401 of Bayer).
The invention has the positive effects that:
1. the silicon dioxide nano-modified polyurethane aqueous dispersion is prepared, and the water-based automobile coating with self-repairing comprehensive performance is prepared.
2. The non-toxic and pollution-free inorganic non-metal nano silicon dioxide is introduced, has a three-dimensional silica structure, is rich in hydrogen bonds on the surface and has stronger activity, the nano modified polyurethane aqueous dispersion for the automobile is prepared, is compounded with the aqueous acrylic dispersion, and is crosslinked and cured to form a film through the hydrophilic modified polyisocyanate, so that a polyurethane network structure with high crosslinking density is formed, has more hydrogen bonds, a main chain of a hard and flexible paint film is deformed but not broken under the external scraping effect, the hydrogen bonds are opened and restored after external force is eliminated and are recombined, some scratches can be found through the observation of the appearance, the main chain is stretched under the stress effect through external input energy (such as sunlight), the hydrogen bonds return to the original positions, the scratches are weakened or disappeared along with the original positions, the self-repairing effect is achieved, and the mechanical strength of the coating is maintained, The decoration effect, the elimination of hidden danger and the extension of service life are of great significance.
3. The nano particles are dispersed in the polymer framework and interact with the framework material, which is beneficial to improving the toughness and mechanical property of the coating. Such as improving the wear resistance, scratch resistance, hardness, strength and the like of the coating, and simultaneously greatly improving the appearance of the paint film, such as luster, leveling property and the like, and the comprehensive performance of the paint film is excellent.
4. The VOC content of the water-based automobile coating product is lower than 10%, the water-based automobile coating product is extremely friendly to the environment, the blank of domestic water-based automobile coatings is filled, energy conservation and emission reduction of automobile coating are realized, and the water-based automobile coating product has a wide market prospect.
Drawings
FIG. 1 is a block diagram of a preparation process of the present invention.
The specific implementation mode is as follows:
example 1
Adding 70 parts by weight of polyethylene glycol, 9 parts by weight of N-methylpyrrolidone and 0.3 part by weight of nano silicon dioxide into a reaction kettle provided with a stirring paddle, a thermometer and a condenser, heating to 80 ℃ under the protection of nitrogen, keeping a high-speed dispersion state for 0.5h, adding 4.5 parts by weight of dimethylolbutyric acid, cooling to 65 ℃, adding 0.03 part by weight of dibutyltin dilaurate and 20 parts by weight of isophorone diisocyanate, keeping the temperature at 80 ℃, continuously reacting for 3.5h, cooling to 55 ℃, adding 3 parts by weight of triethylamine for neutralization, and reacting for 25min until the pH value is 8-9 to obtain the nano modified polyurethane prepolymer aqueous dispersion.
Keeping the prepolymer at 70 ℃, slowly adding the prepolymer into deionized water at 25 ℃ under strong stirring, finally adding a proper amount of ethylenediamine, reacting for 2 hours, and discharging to obtain the silicon dioxide nano-modified polyurethane aqueous dispersion. The performance indexes are as follows:
example 2 Performance indication test method is the same as example 1
Adding 60 parts by weight of polyol (polyethylene glycol, polypropylene glycol or polycarbonate diol, polybutylene adipate diol), 5 parts by weight of N-methylpyrrolidone and 0.1 part by weight of nano silicon dioxide into a reaction kettle provided with a stirring paddle, a thermometer and a condenser, heating to 80 ℃ under the protection of nitrogen, keeping a high-speed dispersion state for 0.5h, adding 3 parts by weight of dimethylolbutyric acid, cooling to 65 ℃, adding 0.02 part by weight of organic tin catalyst (dibutyltin dilaurate, stannous octoate) and 15 parts by weight of polyisocyanate (isophorone diisocyanate or diphenylmethane diisocyanate or hexamethylene diisocyanate), keeping the temperature at 80 ℃, continuously reacting for 3 hours, cooling to 55 ℃, adding 2 parts by weight of neutralizer (ammonia water or triethylamine or dimethylethanolamine) for neutralization, reacting for 25min until the pH value is 8, and obtaining the nano modified polyurethane aqueous dispersion prepolymer.
Keeping the prepolymer at 70 ℃, slowly adding the prepolymer into deionized water at 25 ℃ under strong stirring, finally adding a proper amount of ethylenediamine, reacting for 2 hours, and discharging to obtain the silicon dioxide nano-modified polyurethane aqueous dispersion.
Example 3 Performance indication test method is the same as example 1
Adding 80 parts by weight of polyol (polyethylene glycol, polypropylene glycol or polycarbonate diol, polybutylene adipate diol), 10 parts by weight of N-methyl pyrrolidone and 0.5 part by weight of nano silicon dioxide into a reaction kettle provided with a stirring paddle, a thermometer and a condenser, heating to 80 ℃ under the protection of nitrogen, keeping a high-speed dispersion state for 0.5h, adding 5 parts by weight of dimethylolbutyric acid, cooling to 65 ℃, adding 0.05 part by weight of organic tin catalyst (dibutyltin dilaurate, stannous octoate) and 25 parts by weight of polyisocyanate (isophorone diisocyanate or diphenylmethane diisocyanate or hexamethylene diisocyanate), keeping the temperature at 80 ℃, continuously reacting for 4h, cooling to 55 ℃, adding 4 parts by weight of neutralizer (ammonia water or triethylamine or dimethylethanolamine) for neutralization, reacting for 25min until the pH value is 9 to obtain the nano modified polyurethane aqueous dispersion prepolymer.
Keeping the prepolymer at 70 ℃, stirring strongly, slowly adding the prepolymer into deionized water at 25 ℃, finally adding a proper amount of ethylenediamine, reacting for 2 hours, and discharging to obtain the silicon dioxide nano-modified polyurethane aqueous dispersion.
Example 4: application example of product (taking white as example), preparation of self-repairing type water-based automobile coating and performance index
According to the selectivity research of various raw materials and additives, a self-repairing water-based automobile coating product is prepared (taking white as an example), and the addition amount of each component of a basic formula is as follows:
sequentially adding raw materials, dispersing, grinding and passing the qualification, thus obtaining a finished product of the self-repairing water-based white finish paint for the automobile, namely the component A. And the modified polyisocyanate is uniformly mixed with hydrophilic modified polyisocyanate serving as a component B according to the proportion of A: B and deionized water of 4:1:0.5-1.5 to obtain a finished product capable of being sprayed for construction, wherein the spraying viscosity is 25-30 seconds (coating-4 cups, 25 ℃).
The hydrophilic modified polyisocyanate of the present invention is selected from one or a mixture of modified HDI (Bayhydur 304 of Bayer corporation) and modified IPDI (Bayhydur 401 of Bayer corporation). The following results of the water-based automotive coating were obtained using the test methods commonly used in the coating field:
Claims (6)
1. a method of preparing a ready-to-apply spray automotive coating product, characterized in that the method comprises the steps of: adopting a resin-free milling system, selecting 5-35 parts of water-based pigment, 10-15 parts of deionized water, 0.5-1 part of water-based dispersing agent serving as a functional water-based auxiliary agent and 0.1-0.3 part of water-based defoaming agent, uniformly mixing, grinding the obtained mixture in a water-based sand mill, adding 35-45 parts of silicon dioxide nano modified polyurethane water dispersion, 10-15 parts of water-based acrylic acid dispersion, 0.1-0.3 part of water-based defoaming agent serving as a water-based auxiliary agent, 0.5-0.8 part of thickening agent, 1-5 parts of cosolvent and 0.2-0.4 part of functional rheological auxiliary agent according to a proper proportion under the dispersing condition, and uniformly stirring to prepare a self-repairing water-based automobile coating product serving as a component A; then, uniformly mixing the component A and hydrophilic modified polyisocyanate serving as the component B according to the proportion of the component A to the component B to deionized water of 4:1:0.5-1.5 to obtain a coating product capable of being applied and sprayed;
wherein the aqueous dispersant is Borchi Gen 0451, the aqueous defoamer is BYK024 from Bick, and the aqueous acrylic dispersion is BayHydrol A2601; the thickener is Borchi Gel PW-25, the cosolvent is ethylene glycol butyl ether and propylene glycol methyl ether acetate, and the functional rheological additive is BYK346 from Pico company;
wherein the hydrophilically modified polyisocyanate is one or a mixture of two selected from Bayhydur 304 of Bayer and Bayhydur 401 of Bayer; and
wherein the silicon dioxide nano-modified polyurethane aqueous dispersion is prepared by the following method:
adding 60-80 parts by weight of polyol, 5-10 parts by weight of N-methylpyrrolidone and 0.1-0.5 part by weight of nano-silica into a reaction kettle provided with a stirring paddle, a thermometer and a condenser, heating to 80 ℃ under the protection of nitrogen, keeping a high-speed dispersion state for 0.5h, adding 3-5 parts by weight of dimethylolbutyric acid, cooling to 65 ℃, adding 0.02-0.05 part by weight of organic tin catalyst and 15-25 parts by weight of polyisocyanate, keeping the temperature at 80 ℃, continuously reacting for 3-4h, cooling to 55 ℃, adding 2-4 parts by weight of neutralizer for neutralization, reacting for 25min until the pH value is 8-9, and obtaining the nano-modified polyurethane aqueous dispersion,
keeping the prepolymer at 70 ℃, stirring strongly, slowly adding the prepolymer into deionized water at 25 ℃, finally adding a proper amount of ethylenediamine, reacting for 2 hours, and discharging to obtain the silicon dioxide nano-modified polyurethane aqueous dispersion.
2. The process according to claim 1, wherein the aqueous silica nano-modified polyurethane dispersion is prepared by the following process: adding 70 parts by weight of polyethylene glycol, 9 parts by weight of N-methylpyrrolidone and 0.3 part by weight of nano silicon dioxide into a reaction kettle provided with a stirring paddle, a thermometer and a condenser, heating to 80 ℃ under the protection of nitrogen, keeping a high-speed dispersion state for 0.5h, adding 4.5 parts by weight of dimethylolbutyric acid, cooling to 65 ℃, adding 0.03 part by weight of dibutyltin dilaurate and 20 parts by weight of isophorone diisocyanate, keeping the temperature at 80 ℃, continuously reacting for 3.5h, cooling to 55 ℃, adding 3 parts by weight of triethylamine for neutralization, reacting for 25min until the pH value is 8-9, to obtain the nano modified polyurethane aqueous dispersion prepolymer, keeping the prepolymer at 70 ℃, strongly stirring and slowly adding the prepolymer into deionized water at 25 ℃, finally, adding a proper amount of diethylamine, reacting for 2 hours, and discharging to obtain the silicon dioxide nano-modified polyurethane aqueous dispersion.
3. The method according to claim 1, wherein the polyol is polyethylene glycol, polypropylene glycol or polycarbonate diol or polybutylene adipate diol.
4. The method according to claim 1, wherein the organotin-based catalyst is dibutyltin dilaurate or stannous octoate.
5. The process according to claim 1, wherein the polyisocyanate is isophorone diisocyanate or diphenylmethane diisocyanate or hexamethylene diisocyanate.
6. The process according to claim 1, characterized in that the neutralizing agent is ammonia or triethylamine or dimethylethanolamine.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711026375.5A CN108070318B (en) | 2017-10-26 | 2017-10-26 | Preparation method and application of self-repairing water-based automobile coating |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711026375.5A CN108070318B (en) | 2017-10-26 | 2017-10-26 | Preparation method and application of self-repairing water-based automobile coating |
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| Publication Number | Publication Date |
|---|---|
| CN108070318A CN108070318A (en) | 2018-05-25 |
| CN108070318B true CN108070318B (en) | 2022-09-23 |
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| CN109575223A (en) * | 2018-12-28 | 2019-04-05 | 南京高正农用化工有限公司 | A kind of temperature and pH stimuli-responsive intelligent polymer microcapsule and preparation method thereof |
| CN114213965B (en) * | 2021-12-31 | 2022-11-11 | 清远华湾材料研究院有限公司 | Automobile finish paint and preparation method thereof |
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| CN101294045A (en) * | 2007-04-25 | 2008-10-29 | 朱斌 | Method for producing watersoluble floating coat paint suitable for original factory of vehicle and repair |
| CN102153984A (en) * | 2011-01-26 | 2011-08-17 | 山西省应用化学研究所 | Method for preparing single-component high-heat-resistance aqueous polyurethane adhesive |
| CN103613730A (en) * | 2013-11-21 | 2014-03-05 | 五邑大学 | Method for preparing high-solid content waterborne polyurethane by using nano silicon dioxide polyether (ester) polyalcohol dispersion |
| CN104695231A (en) * | 2015-03-09 | 2015-06-10 | 东南大学 | Waterproof moisture-permeable waterborne polyurethane fabric coating material and preparation method thereof |
| CN107236114A (en) * | 2017-06-15 | 2017-10-10 | 盐城工学院 | A kind of watersoluble closed type polyisocyanate crosslinking agent of nano-silica-containing structure and preparation method thereof |
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| CN101294045A (en) * | 2007-04-25 | 2008-10-29 | 朱斌 | Method for producing watersoluble floating coat paint suitable for original factory of vehicle and repair |
| CN102153984A (en) * | 2011-01-26 | 2011-08-17 | 山西省应用化学研究所 | Method for preparing single-component high-heat-resistance aqueous polyurethane adhesive |
| CN103613730A (en) * | 2013-11-21 | 2014-03-05 | 五邑大学 | Method for preparing high-solid content waterborne polyurethane by using nano silicon dioxide polyether (ester) polyalcohol dispersion |
| CN104695231A (en) * | 2015-03-09 | 2015-06-10 | 东南大学 | Waterproof moisture-permeable waterborne polyurethane fabric coating material and preparation method thereof |
| CN107236114A (en) * | 2017-06-15 | 2017-10-10 | 盐城工学院 | A kind of watersoluble closed type polyisocyanate crosslinking agent of nano-silica-containing structure and preparation method thereof |
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