CN113321996B - Fluorine modified weather-proof solvent-free elastic coating and preparation method thereof - Google Patents
Fluorine modified weather-proof solvent-free elastic coating and preparation method thereof Download PDFInfo
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- CN113321996B CN113321996B CN202011625400.3A CN202011625400A CN113321996B CN 113321996 B CN113321996 B CN 113321996B CN 202011625400 A CN202011625400 A CN 202011625400A CN 113321996 B CN113321996 B CN 113321996B
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- 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
- C08K3/20—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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- Polyurethanes Or Polyureas (AREA)
Abstract
The invention relates to a fluorine modified weather-proof solvent-free elastic coating and a preparation method thereof. The novel fluorine modified weather-proof solvent-free elastic coating comprises a first component and a second component, wherein the first component is composed of an isocyanate prepolymer formed by reacting aliphatic isocyanate with a hydroxyl acrylate monomer, a catalyst, fluorine-containing acrylate, a cross-linking agent and high-molecular dihydric alcohol, and the second component is composed of a chain extender, fatty amine, a pigment, a dispersing agent and an auxiliary agent. The coating has high strength and good flexibility, does not contain VOC, is more weather-resistant, acid-base-resistant, solvent-resistant, contamination-resistant and high-temperature-resistant than common solvent-free elastic coatings, and is very suitable for outdoor long-term protection of water resistance, corrosion resistance, pollution resistance, impact resistance and the like.
Description
Technical Field
The invention relates to a technology of fluorine modified weather-proof solvent-free elastic coating.
Background
The conventional solvent-free elastomeric coatings have the following disadvantages:
common solvent-free elastic coatings are mainly of two main types, namely polyurethane and polyurea, but all of the common solvent-free elastic coatings contain a large number of aromatic groups and ether bonds, so that the common solvent-free elastic coatings are easy to discolor and have poor weather resistance and chemical resistance. For example, it discolors for several days outdoors, loses light seriously for several months, and it is easily swelled by a solvent.
The common fluorocarbon coating has the following advantages:
(1) excellent corrosion resistance-thanks to excellent chemical inertness, the paint film is resistant to chemicals such as acids, bases, salts and various chemical solvents, providing a protective barrier for the substrate. The paint film is tough, high in surface hardness, impact resistant, buckling resistant and good in wear resistance. Exhibit excellent physical and mechanical properties.
(2) The fluorocarbon coating has extremely low surface energy, surface dust can be self-cleaned by rainwater, excellent hydrophobicity (the maximum water absorption is less than 5 percent) and oil repellency, extremely small friction coefficient (0.15-0.17), no dust adhesion and scaling and good antifouling property.
(3) And strong adhesion, namely, the adhesive has excellent adhesion on the surfaces of metals such as copper, stainless steel and the like, plastics such as polyester, polyurethane, vinyl chloride and the like, cement, composite materials and the like, and basically shows the characteristic of being suitable for being attached to any material. High decorative effect, namely, in a 60-degree gloss meter, the high gloss of more than 80 percent can be achieved.
(4) The coating has a large amount of F-C bonds, strong bond energy determines the super-strong stability, and the coating does not chalk and fade, has a service life as long as 20 years, and has more excellent service performance than any other coating. Excellent application property-double component package, long storage period and convenient application.
But also has significant disadvantages:
contains a certain amount of various solvents, both aqueous and oily, and is not good in environmental protection.
Lack of elasticity, generally very low elasticity, and limited application.
The film is thin and difficult to be coated thickly.
Aiming at the problem, the invention introduces fluorine on the elastic chain segment by using a fluorine modification method, introduces the advantages of fluorine, removes the original defects of the fluorine coating, uses weather-resistant aliphatic isocyanate and aliphatic amine, improves the weather resistance, high temperature resistance, solvent resistance and stain resistance of the coating, uses a fluorine surfactant and further improves the stain resistance.
Disclosure of Invention
The invention aims to provide a novel fluorine modified weather-proof solvent-free elastic coating and a preparation method thereof. According to one aspect of the invention, the novel fluorine modified weather-proof solvent-free elastic coating comprises a first component and a second component, wherein the first component is composed of an isocyanate prepolymer formed after reaction of aliphatic isocyanate, a hydroxyl acrylate monomer, a catalyst, fluorine-containing acrylate, a cross-linking agent and high molecular diol, and the second component is composed of a chain extender, aliphatic amine, a pigment, a dispersing agent and an auxiliary agent.
The novel fluorine modified weather-proof solvent-free elastic coating is characterized in that the isocyanate is one or more of hexamethylene diisocyanate or isophorone diisocyanate and hydrogenated phenyl methane diisocyanate.
The novel fluorine modified weather-resistant solvent-free elastic coating is characterized in that the catalyst is organic bismuth and azodiisobutyronitrile.
The novel fluorine modified weather-resistant solvent-free elastic coating is characterized in that the hydroxyl acrylate monomer is hydroxyethyl acrylate or hydroxypropyl acrylate.
The novel fluorine-modified weather-resistant solvent-free elastic coating is characterized in that the fluorine-containing acrylate is hexafluorobutyl acrylate.
The novel fluorine modified weather-resistant solvent-free elastic coating is characterized in that the crosslinking agent is trimethylolpropane.
The novel fluorine modified weather-proof solvent-free elastic coating is characterized in that the high-molecular dihydric alcohol is polycarbonate dihydric alcohol or polycaprolactone polyol with the molecular weight of 1000-3000.
The novel fluorine modified weather-resistant solvent-free elastic coating is characterized in that the chain extender is isophorone diamine or diethylene triamine.
The novel fluorine modified weather-resistant solvent-free elastic coating is characterized in that the aliphatic amine is Epikure 3292-FX-60.
The novel fluorine modified weather-proof solvent-free elastic coating is characterized in that the pigment is one or more of pearlescent powder, carbon black, iron oxide red, titanium dioxide and the like.
The novel fluorine modified weather-proof solvent-free elastic coating is characterized in that the dispersing agent is a solvent-free high-molecular dispersing agent.
The novel fluorine modified weather-proof solvent-free elastic coating is characterized in that the auxiliary agent is a fluorine surfactant.
According to another aspect of the present disclosure, there is also provided a method for preparing a novel fluorine-modified weather-resistant solvent-free elastomeric coating, comprising: vacuumizing a reaction kettle, filling nitrogen, adding 20-50 parts of isocyanate, adding 0.1-0.5 part of catalyst at the rotation speed of 60-80 revolutions per minute, adding 2-12 parts of hydroxyl acrylate monomer, filling nitrogen, heating to 65-70 ℃, reacting for 4-5 hours, adding another catalyst, adding 5-24 parts of fluorine-containing acrylate by a dropwise adding method, completing the dropwise addition within 1-1.5 hours, reacting for 3-4 hours, then adding 0.5-5 parts of cross-linking agent and 20-40 parts of high-molecular dihydric alcohol, raising the temperature to 80 ℃, continuing to react for 2-4 hours, cooling to 55-60 ℃, and finishing the preparation of the first component; and adding 10-40 parts of isophorone diamine chain extender, 40-60 parts of aliphatic amine Epikure3292-FX-60, 0.2-5 parts of dispersing agent, rotating speed of 600 and 1000 revolutions per minute, dispersing for 5 minutes, adding 3-15 parts of pigment, 0.1-1 part of fluorine surfactant, rotating speed of 3000-4000 revolutions per minute, dispersing for 2-3 hours, stopping the machine, and finishing the preparation of the second component. .
Detailed Description
The invention is further described below with reference to specific examples.
The specific implementation mode is as follows:
the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention is realized by the following technical scheme:
preparation of the first component (in parts by mass hereinafter)
Vacuumizing a reaction kettle, filling nitrogen, adding 35-65 parts of isocyanate, adding 0.1-0.5 part of catalyst at the rotation speed of 60-80 revolutions per minute, adding 2-12 parts of hydroxyl acrylate monomer, filling nitrogen, heating to 65-70 ℃, reacting for 4-5 hours, adding 0.1-0.5 part of another catalyst, adding 5-24 parts of fluorine-containing acrylate by adopting a dropwise adding method, finishing dropping within 1-1.5 hours, reacting for 3-4 hours, then adding 0.5-5 parts of cross-linking agent and 20-40 parts of high molecular dihydric alcohol, raising the temperature to 80 ℃, continuing to react for 2-4 hours, cooling to 55-60 ℃, and finishing the preparation of the first component.
Preparation of the second component
The novel fluorine modified weather-resistant polyurea coating material as claimed in claim 1, wherein the second component is prepared by adding 10-40 parts of isophorone diamine chain extender, 40-60 parts of aliphatic amine Epikure3292-FX-60, 0.2-5 parts of dispersant, at a rotation speed of 600-.
In a preferred embodiment of the invention, the isocyanate is isophorone diisocyanate.
In a preferred embodiment of the present invention, the catalyst is organobismuth and azobisisobutyronitrile.
In a preferred embodiment of the present invention, the hydroxy acrylate monomer is hydroxyethyl acrylate.
In a preferred embodiment of the present invention, the fluoroacrylate is hexafluorobutyl acrylate.
In a preferred embodiment of the invention, the cross-linking agent is trimethylolpropane.
In a preferred embodiment of the present invention, the polymer diol is a polycarbonate diol having a molecular weight of 2000.
In a preferred embodiment of the invention, the chain extender is isophoronediamine.
In a preferred embodiment of the invention, the aliphatic amine is Epikure 3292-FX-60.
In a preferred embodiment of the invention, the pigment is one or more of pearlescent powder, carbon black, iron oxide red, titanium dioxide and the like.
In a preferred embodiment of the present invention, the dispersant is a solvent-free polymeric dispersant 6320.
In a preferred embodiment of the invention, the adjuvant is a fluorosurfactant 6215.
Example 1 preparation of paint 1 (Gray) (in parts by mass below)
Preparation of the first component
Vacuumizing a reaction kettle, filling nitrogen, adding 55 parts of isophorone diisocyanate, adding 0.2 part of catalyst organic bismuth at the rotation speed of 60-80 rpm, adding 4 parts of hydroxy acrylate hydroxyethyl ester monomer, filling nitrogen, heating to 65-70 ℃, reacting for 4 hours, adding 0.1 part of another catalyst azodiisobutyronitrile, adding 8 parts of hexafluorobutyl acrylate by a dropwise adding method, completing the dropwise addition within 1 hour, reacting for 3 hours, then adding 2 parts of cross-linking agent trimethylolpropane and 30.7 parts of 2000 molecular weight polycarbonate diol, raising the temperature to 80 ℃, continuing the reaction for 3 hours, cooling to 55-60 ℃, and finishing the preparation of the first component.
Preparation of the second component
Adding 32 parts of isophorone diamine chain extender, 50 parts of aliphatic amine Epikure3292-FX-60, 3 parts of dispersing agent 6320, rotating speed of 700 rpm, dispersing for 5 minutes, adding 14.4 parts of titanium dioxide, 0.1 part of carbon black, adding 0.5 part of fluorine surfactant 6215, rotating speed of 3500 rpm, dispersing for 3 hours, stopping the machine, and finishing the preparation of the second component.
Example 2 preparation of dope 2 (iron red) (hereinafter, all in parts by mass)
Preparation of the first component
Vacuumizing a reaction kettle, filling nitrogen, adding 57 parts of isophorone diisocyanate, adding 0.2 part of catalyst organic bismuth at the rotation speed of 60-80 revolutions per minute, adding 4 parts of hydroxy acrylate hydroxyethyl ester monomer, filling nitrogen, heating to 65-70 ℃, reacting for 4 hours, adding 0.1 part of another catalyst azodiisobutyronitrile, adding 8 parts of hexafluorobutyl acrylate by a dropwise adding method, completing the dropwise addition within 1 hour, reacting for 3 hours, then adding 2 parts of cross-linking agent trimethylolpropane and 28.7 parts of 2000 molecular weight polycarbonate diol, raising the temperature to 80 ℃, continuing the reaction for 3 hours, cooling to 55-60 ℃, and finishing the preparation of the first component.
Preparation of the second component
Adding 35 parts of isophorone diamine chain extender, 52 parts of aliphatic amine Epikure3292-FX-60, 2 parts of dispersing agent 6320, rotating at 700 rpm, adding 10.6 parts of iron oxide red, dispersing for 5 minutes, adding 0.4 part of fluorine surfactant 6215, rotating at 35000 rpm, dispersing for 3 hours, stopping the machine, and finishing the preparation of the second component
The test results for the DF-20/35A device spray pattern of the first and second examples, Dongsheng Futian, were as follows:
example 1 and example 2 comparison of coating spray pattern performance parameters
From the comparison results, it can be seen that the tensile strength, the elongation at break, the tear strength and other properties of the materials in example 1 and example 2 are obviously different when the material proportions are different.
The above embodiments are merely illustrative of the present disclosure and do not represent a limitation of the present disclosure. Other variations of the embodiments of the invention will occur to those skilled in the art.
Claims (12)
1. A fluorine modified weather-proof solvent-free elastic coating comprises a first component and a second component, wherein the first component is composed of an isocyanate prepolymer formed by reacting aliphatic isocyanate with a hydroxyl acrylate monomer, a catalyst, fluorine-containing acrylate, a cross-linking agent and high molecular dihydric alcohol, the second component is composed of a chain extender, fatty amine, a pigment, a dispersant and an auxiliary agent,
the first component is prepared through vacuumizing in a reactor, introducing nitrogen, adding isocyanate in 20-50 weight portions, adding catalyst organic bismuth in 0.1-0.5 weight portion at 60-80 rpm, adding hydroxyl acrylate monomer in 2-12 weight portions, introducing nitrogen, heating to 65-70 deg.c to react for 4-5 hr, adding azodiisobutyronitrile as the other catalyst, adding fluoro acrylate in 5-24 weight portions through dropping for 1-1.5 hr to react for 3-4 hr, adding cross-linking agent in 0.5-5 weight portions, adding polymer glycol in 20-40 weight portions, heating to 80 deg.c, further reacting for 2-4 hr, and cooling to 55-60 deg.c to complete the preparation.
2. The fluorine modified weather-resistant solvent-free elastic coating as claimed in claim 1, wherein the isocyanate is one or more of hexamethylene diisocyanate or isophorone diisocyanate, and hydrogenated phenyl methane diisocyanate.
3. The fluorine modified weather resistant solventless elastomeric coating of claim 1 wherein the hydroxy acrylate monomer is hydroxyethyl acrylate or hydroxypropyl acrylate.
4. The fluorine modified weather resistant solventless elastomeric coating of claim 1 wherein the fluoroacrylate is hexafluorobutyl acrylate.
5. The fluorine modified weather resistant solventless elastomeric coating of claim 1 wherein the crosslinking agent is trimethylolpropane.
6. The fluorine modified weather-resistant solvent-free elastic coating as claimed in claim 1, wherein the polymer diol is polycarbonate diol or polycaprolactone polyol with molecular weight of 1000-3000.
7. The fluorine modified weather resistant solventless elastomeric coating of claim 1 wherein the chain extender is isophorone diamine or diethylene triamine.
8. The fluorine-modified weather-resistant solvent-free elastomeric coating of claim 1, wherein the aliphatic amine is Epikure 3292-FX-60.
9. The fluorine modified weather-resistant solvent-free elastic coating as claimed in claim 1, wherein the pigment is one or more of pearlescent powder, carbon black, iron oxide red and titanium dioxide pigment.
10. The fluorine modified weather-resistant solvent-free elastomeric coating of claim 1, wherein the dispersant is a solvent-free polymeric dispersant.
11. The fluorine modified weather-resistant solvent-free elastomeric coating of claim 1, wherein the auxiliary agent is a fluorosurfactant.
12. A method of preparing a fluorine modified weatherable, solvent-free elastomeric coating comprising:
vacuumizing a reaction kettle, filling nitrogen, adding 20-50 parts of isocyanate, adding 0.1-0.5 part of catalyst organic bismuth at the rotation speed of 60-80 revolutions per minute, adding 2-12 parts of hydroxyl acrylate monomer, filling nitrogen, heating to 65-70 ℃, reacting for 4-5 hours, adding another catalyst azodiisobutyronitrile, adding 5-24 parts of fluorine-containing acrylate by adopting a dropwise adding method, finishing dropping within 1-1.5 hours, reacting for 3-4 hours, then adding 0.5-5 parts of cross-linking agent and 20-40 parts of high molecular dihydric alcohol, raising the temperature to 80 ℃, continuing to react for 2-4 hours, cooling to 55-60 ℃, and finishing the preparation of the first component; and
adding 10-40 parts of isophorone diamine chain extender, 40-60 parts of aliphatic amine Epikure3292-FX-60 into a dispersion tank, adding 0.2-5 parts of dispersant, rotating at the speed of 600 revolutions per minute, dispersing for 5 minutes, adding 3-15 parts of pigment, 0.1-1 part of fluorine surfactant, rotating at the speed of 3000-4000 revolutions per minute, dispersing for 2-3 hours, stopping the machine, and finishing the preparation of the second component.
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| CN104744651A (en) * | 2015-02-15 | 2015-07-01 | 陕西科技大学 | Environment-friendly fluorinated polyurethane-polyacrylate emulsion and preparation method thereof |
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| CN106010175B (en) * | 2016-07-05 | 2018-02-23 | 江苏苏博特新材料股份有限公司 | A kind of preparation method and applications of bridge anti-freezing ice type two-component polyurea water-repellent paint |
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| CN104744651A (en) * | 2015-02-15 | 2015-07-01 | 陕西科技大学 | Environment-friendly fluorinated polyurethane-polyacrylate emulsion and preparation method thereof |
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Effective date of registration: 20220310 Address after: 053499 workshop 1, Hebei Daocheng logistics park, Circular Economy Park, high tech Zone, Hengshui City, Hebei Province Patentee after: Hebei shuaikuoda New Material Technology Co.,Ltd. Address before: No. 905, floor 9, Yuquan building, No. 3, Shijingshan Road, Shijingshan District, Beijing 100049 Patentee before: Beijing Kuo Shuai new materials Co.,Ltd. |