CN110408291B - Fluorine-containing aqueous self-layering coating and preparation method thereof - Google Patents
Fluorine-containing aqueous self-layering coating and preparation method thereof Download PDFInfo
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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
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- C09D143/00—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 containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Coating compositions based on derivatives of such polymers
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- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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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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- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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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
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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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Abstract
The invention provides a fluorine-containing aqueous self-layering coating, which comprises the following components in percentage by weight: 10 to 60 percent of fluorine-containing water-based resin, 10 to 60 percent of fluorine-free water-based resin, 0.5 to 20 percent of auxiliary agent for water-based paint, 0 to 30 percent of film-forming auxiliary agent and 20 to 70 percent of deionized water; the fluorine-containing waterborne self-layering coating can ensure the stability of the self-layered coating, thereby ensuring the substrate adhesive force and the water, oil and stain resistance of the coating, and the coating is waterborne and has good environmental protection performance. The invention also provides a preparation method of the fluorine-containing aqueous self-layering coating.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a fluorine-containing aqueous self-layering coating and a preparation method thereof.
Background
With the development of modern industry, more and more substrates have not only limited to beauty, but also put forward the protection requirement of surface functionalization, wherein, the fluorine-containing low surface energy coating which improves the water, oil and dirt repellency of the surface of a coating film is one of the most widely applied coatings with the largest application requirement in the existing coating field. However, the fluorine-containing low surface energy coating has the problems of poor spreading and wetting, poor adhesion, high cost and the like on the surface of a coated substrate due to low surface energy, and is limited and influenced in the process of popularization and application.
The self-layering technology is characterized in that coating materials with different surface energies and different electronegativities are coated on the surface of a base material, and the coating materials are spontaneously layered by utilizing the difference of the surface energies of the coating materials, so that the coating materials with low surface energies are gathered on the surface of a coating, and the coating materials with high surface energies are attached to the surface of a matrix, so that the whole coating material has good adhesive force and strong water, oil and dirt repellency.
However, in practical application, it is found that the stability of the self-layering coating is poor, the movement of the fluorine-containing chain segment of the surface layer often causes the surface layer to slump, so that the water-repellent, oil-repellent and dirt-repellent capabilities of the surface layer are deteriorated, the collapsed fluorine-containing chain segment also affects the adhesion capability of the fluorine-free resin of the bottom layer, so that the adhesion force of the whole coating on a substrate is deteriorated with the passage of time, the application effect is further deteriorated, and the actual requirement is difficult to meet.
Therefore, the preparation of an aqueous fluorine-containing coating with both excellent substrate adhesion and excellent surface properties is an urgent need in the field.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the fluorine-containing aqueous self-layering coating and the preparation method thereof, which can ensure the stability of the coating after self-layering, thereby ensuring that the coating has excellent substrate adhesive force and excellent surface water, oil and dirt repellent capabilities.
In order to achieve the above purpose, the solution adopted by the invention is as follows: a fluorine-containing aqueous self-layering coating comprises the following components in percentage by weight: 10 to 60 percent of fluorine-containing water-based resin, 10 to 60 percent of fluorine-free water-based resin, 0.5 to 20 percent of auxiliary agent for water-based paint, 0 to 30 percent of film-forming auxiliary agent and 20 to 70 percent of deionized water; the structure of the fluorine-containing water-based resin is shown as a formula I, and a silane coupling agent is copolymerized in the fluorine-free water-based resin
Preferably, the fluorine-containing aqueous self-layering coating comprises the following components in percentage by weight: 15-35% of fluorine-containing water-based resin, 20-40% of fluorine-free water-based resin, 1-10% of water-based paint auxiliary agent, 10-25% of film-forming auxiliary agent and 20-40% of deionized water.
Preferably, the fluorine-containing aqueous self-layering coating comprises the following components in percentage by weight: 19-31% of fluorine-containing water-based resin, 25-37% of fluorine-free water-based resin, 2-6% of water-based paint auxiliary agent, 14-20% of film-forming auxiliary agent and 20-25% of deionized water.
The self-layering process of the fluorine-containing aqueous self-layering coating is shown in the attached figure 1, in the drying and film-forming process of the coating, the fluorine-containing aqueous resin with low surface energy can automatically migrate to the surface under the pulling of a fluorine-containing chain segment, so that the fluorine-containing aqueous resin with low surface energy is gathered on the surface, excellent surface water repellency, oil repellency and dirt repellency are obtained, meanwhile, the surface energy is relatively high, and the fluorine-free aqueous resin containing a silane coupling agent is gathered on the bottom layer and well spreads and adheres to the surface of a matrix.
As shown in the formula I, the fluorine-containing water-based resin is a fluorine-containing water-based resin with an umbrella-shaped structure, the fluorine-containing water-based resin with the umbrella-shaped structure is formed by emulsion polymerization of an acrylate monomer and a fluorine-containing short chain compound monomer with the umbrella-shaped structure, the umbrella-shaped structure of the fluorine-containing water-based resin covers the surface of polyacrylate, and due to the increase of the steric hindrance of the umbrella-shaped structure, a fluorine chain can stably cover the surface, so that the problem of chain segment collapse cannot occur; in addition, the fluorine-free water-based resin is copolymerized with the silane coupling agent, and the adhesive force between the fluorine-free water-based resin and the surface of the base material is improved by utilizing the principle that the siloxy group of the silane coupling agent has reactivity to inorganic matters and the organic functional group has reactivity to organic matters; the two materials have synergistic effect, so that the low-surface-energy fluorine-containing resin can automatically migrate to the surface and stably exists on the surface, and the high-surface-energy fluorine-free water-based resin can stably exist on the bottom surface and well adheres to the base material, so that the surface obtains excellent water and oil repellency and stain repellency, and the bottom surface has excellent adhesion.
Specifically, the preparation method of the fluorine-containing water-based resin comprises the following steps: mixing 4-25 wt% of acrylate monomer, 5-15 wt% of umbrella-shaped short-chain fluorine-containing compound monomer, surfactant, initiator and water, and emulsifying at high speed to form pre-emulsion; putting part of the pre-emulsion into a flask, stirring and refluxing at 50-65 ℃ for reaction for 0.5-1.5 h; dropwise adding the rest of the pre-emulsion into the reaction system for 2-5 h; keeping the temperature and reacting for 2-5 h; cooling and filtering to obtain the final fluorine-containing water-based resin emulsion. The preparation method of the fluorine-free water-based resin comprises the following steps: mixing fluorine-free water-based resin monomer (20-35 wt%), silane coupling agent monomer (0.1-2.0 wt%), surfactant, initiator and water, and emulsifying at high speed to form pre-emulsion; putting part of the pre-emulsion into a flask, stirring and refluxing at 50-85 ℃ for reaction for 0.5-1.5 h; dropwise adding the rest of the pre-emulsion into the reaction system for 2-5 h; keeping the temperature and reacting for 2-5 h; cooling and filtering to obtain the final fluorine-free aqueous resin emulsion.
The preparation methods of the fluorine-containing water-based resin and the fluorine-free water-based resin are conventional emulsion polymerization methods.
Preferably, the fluorine-containing water-based self-layering coating also comprises 0.4 to 3 weight percent of water-based blocked isocyanate. Preferably, the weight percentage of the water-based blocked isocyanate is 0.4-1.3%. The fluorine-containing aqueous self-layering coating disclosed by the invention is automatically layered in the heating and drying process, after layering, isocyanate in the coating is taken as a cross-linking agent, and under the heating action, the fluorine-containing aqueous resin on the surface layer and the fluorine-free aqueous resin on the bottom layer are cross-linked and cured, so that the combination of the fluorine-containing aqueous resin and the fluorine-free aqueous resin is more stable, the connection stability between the layers is ensured, and the collapse of a fluorine-containing chain segment to the bottom layer is further avoided.
Preferably, the silane coupling agent monomer is at least one of gamma-aminopropyltriethoxysilane (KH550), gamma-glycidoxypropyltrimethoxysilane (KH560) and gamma- (methacryloyloxy) propyltrimethoxysilane (KH 570).
Preferably, the fluorine-free water-based resin is one or more of water-based polyacrylate resin, water-based polyurethane-polyacrylate composite resin and water-based epoxy resin.
Preferably, the auxiliary agent for the water-based paint is one or more of a wetting agent, a dispersing agent, a defoaming agent, a leveling agent, a thickening agent, a preservative and a mildew preventive.
Preferably, the coalescent is an organic solvent and the coalescent is miscible with water. Preferably, the film forming aid is one or more of propylene glycol butyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether and dipropylene glycol butyl ether.
The preparation method of the fluorine-containing aqueous self-layering coating comprises the following steps: adding part of water, a film-forming assistant and a defoaming agent into a mixing tank, and uniformly stirring; then adding fluorine-containing water-based resin and fluorine-free water-based resin, and uniformly stirring; then adding the flatting agent, the thickening agent, the preservative, the mildew preventive and the water-based closed isocyanate in sequence, and stirring uniformly; adjusting the viscosity and the pH value, and adjusting the pH value to 6-7; filtering and discharging to obtain the fluorine-containing water-based self-layering coating.
The invention has the beneficial effects that:
(1) according to the fluorine-containing aqueous self-layering coating, the fluorine-containing aqueous resin moves towards the surface layer under the pulling of the fluorine-containing chain segment, and the fluorine-containing chain segment is ensured to be stabilized on the surface layer due to the shielding effect of the umbrella-shaped structure; the silane coupling agent copolymerized with the fluorine-free water-based resin promotes the fluorine-free water-based resin to be better attached to the surface of the matrix; the addition of isocyanate enables the fluorine-containing water-based resin and the fluorine-free water-based resin to be crosslinked and cured after layering, and the formed layered structure is further stable; the above functions enable different coating materials to form a stable layered structure, the condition of interlayer collapse is avoided, and the water repellency, oil repellency and dirt repellency of the surface layer and the good adhesion performance of the bottom layer are effectively ensured.
(2) The fluorine-containing aqueous self-layering coating is formed by mixing the fluorine-containing aqueous resin with the umbrella-shaped structure and the fluorine-free aqueous resin, and the short-chain fluorine-containing aqueous resin with the umbrella-shaped structure has excellent water repellency, oil repellency and dirt repellency due to the shielding effect of the short-chain fluorine-containing aqueous resin, does not need to use long-chain solvent type fluorine-containing resin, and has excellent environmental protection performance and lower cost.
Drawings
FIG. 1 is a self-stratifying process of a fluorine-containing aqueous self-stratifying coating.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The fluorine-containing aqueous self-laminating coating and the preparation method thereof according to the present invention will be further described with reference to the following examples.
The dispersant, wetting agent, defoaming agent, leveling agent, thickener, preservative, antifungal agent, etc. in the following examples can be commercially available to obtain a finished product. The fluorine-containing aqueous resin and the fluorine-free aqueous resin in the following examples were prepared by the production methods described in the summary of the invention.
Example 1
The embodiment provides a preparation method of a fluorine-containing water-based acrylate low-surface-energy self-layering coating for plastic surfaces, which comprises the following steps:
(1) 0.2kg of wetting agent (TRITON), 0.2kg of dispersant (Flowen D-90) and 0.2kg of defoamer (024) were added to an aqueous medium composed of 10.0kg of water and 8.0kg of film-forming aid (propylene glycol butyl ether) in a vessel with a stirrer, and stirred for 30 minutes;
(2) then 10.0kg of fluorine-containing water-based resin with an umbrella-shaped structure and 10.0kg of water-based acrylate resin containing a coupling agent (KH550) are added into the mixture, and stirred for 40 minutes;
(3) then, 0.2kg of thickening agent (sodium polyacrylate), 0.1kg of Preservative (PT), 0.2kg of mildew preventive (sodium pentachlorophenate) and 0.5g of water-based blocked isocyanate are added in sequence and stirred for 20 minutes;
(4) adjusting the pH value to prepare the aqueous fluorine-containing self-layering coating which can be used on the surfaces of plastic parts such as PVC, PS and the like.
Example 2
The embodiment provides a preparation method of a water-based fluorine-containing polyurethane low-surface-energy self-layering coating for a woodware surface, which comprises the following steps:
(1) in a container with a stirrer, 0.2kg of wetting agent (TRITON), 0.2kg of dispersing agent (Flowen D-90) and 0.5kg of defoaming agent (JC-1) are added into an aqueous medium consisting of 10.0kg of water and 6.0kg of film-forming additive (dipropylene glycol butyl ether), and stirred for 30 minutes;
(2) then 8.0kg of fluorine-containing aqueous resin with an umbrella-shaped structure and 15.0kg of aqueous polyurethane resin containing a coupling agent (KH570) are added into the mixture, and stirred for 60 minutes;
(3) then adding 0.2kg of thickening agent (polyvinylpyrrolidone), 0.1kg of preservative (MB-11), 0.5kg of mildew preventive (METATIN55-21), 0.5kg of brightener and 0.2g of water-based blocked isocyanate in sequence, and stirring for 30 minutes;
(4) adjusting the pH value to prepare the aqueous fluorine-containing self-layering coating for the wood surface.
Example 3
The embodiment provides a preparation method of a water-based fluorine-containing epoxy low-surface-energy self-layering coating for metal surfaces, which specifically comprises the following steps:
(1) 1.0kg of wetting dispersant (Atsurf3222) and 0.5kg of defoaming agent (JC-1) were added to an aqueous medium composed of 8.0kg of water and 6.0kg of film-forming aid (propylene glycol monomethyl ether) in a vessel with a stirrer, and stirred for 30 minutes;
(2) then adding 12.0kg of fluorine-containing water-based resin with an umbrella-shaped structure and 10.0kg of water-based epoxy resin containing a coupling agent KH550 into the mixture, and stirring for 40 minutes;
(3) then adding 0.3kg of thickening agent (poly montmorillonite), 0.1kg of Preservative (PT), 0.4kg of mildew preventive (METATIN55-21) and 0.5g of water-based blocked isocyanate in sequence, and stirring for 30 minutes;
(4) adjusting the pH value to prepare the aqueous fluorine-containing self-layering coating which can be used on the surfaces of aluminum materials, steel materials and other metals.
Example 4
The embodiment provides a preparation method of a fluorine-containing water-based acrylate low-surface-energy self-layering coating for plastic surfaces, which comprises the following steps:
(1) 0.2kg of wetting agent (TRITON), 0.2kg of dispersant (Flowen D-90) and 0.2kg of defoamer (024) were added to an aqueous medium composed of 17.0kg of water and 5.0kg of film-forming aid (propylene glycol butyl ether) in a vessel with stirring, and stirred for 30 minutes;
(2) then 21.0kg of fluorine-containing aqueous resin with an umbrella-shaped structure and 6.0kg of aqueous acrylate resin containing a coupling agent (KH550) are added into the mixture, and stirred for 40 minutes;
(3) then, 0.2kg of thickening agent (sodium polyacrylate), 0.1kg of Preservative (PT), 0.2kg of mildew preventive (sodium pentachlorophenate) and 1.5g of water-based blocked isocyanate are added in sequence and stirred for 20 minutes;
(4) adjusting the pH value to prepare the aqueous fluorine-containing self-layering coating which can be used on the surfaces of plastic parts such as PVC, PS and the like.
Example 5
The embodiment provides a preparation method of a water-based fluorine-containing polyurethane low-surface-energy self-layering coating for a woodware surface, which comprises the following steps:
(1) in a container with a stirrer, 0.2kg of wetting agent (TRITON), 0.2kg of dispersing agent (Flowen D-90) and 0.5kg of defoaming agent (JC-1) are added into an aqueous medium consisting of 10.0kg of water and 18.0kg of film-forming additive (dipropylene glycol butyl ether), and stirred for 30 minutes;
(2) then 8.0kg of fluorine-containing aqueous resin with an umbrella-shaped structure and 21.0kg of aqueous polyurethane resin containing a coupling agent (KH570) are added into the mixture, and stirred for 60 minutes;
(3) then adding 0.2kg of thickening agent (polyvinylpyrrolidone), 0.1kg of preservative (MB-11), 0.5kg of mildew preventive (METATIN55-21), 0.5kg of brightener and 1.0g of water-based blocked isocyanate in sequence, and stirring for 30 minutes;
(4) adjusting the pH value to prepare the aqueous fluorine-containing self-layering coating for the wood surface.
Example 6
The embodiment provides a preparation method of a water-based fluorine-containing epoxy low-surface-energy self-layering coating for metal surfaces, which specifically comprises the following steps:
(1) 1.0kg of wetting dispersant (Atsurf3222) and 0.5kg of defoaming agent (JC-1) were added to an aqueous medium composed of 10.0kg of water and 6.0kg of film-forming aid (propylene glycol monomethyl ether) in a vessel with a stirrer, and stirred for 30 minutes;
(2) then adding 13.0kg of fluorine-containing water-based resin with an umbrella-shaped structure and 13.0kg of water-based epoxy resin containing a coupling agent KH550 into the mixture, and stirring for 40 minutes;
(3) then adding 0.3kg of thickening agent (poly montmorillonite), 0.1kg of Preservative (PT), 0.4kg of mildew preventive (METATIN55-21) and 0.5g of water-based blocked isocyanate in sequence, and stirring for 30 minutes;
(4) adjusting the pH value to prepare the aqueous fluorine-containing self-layering coating which can be used on the surfaces of aluminum materials, steel materials and other metals.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The fluorine-containing aqueous self-layering coating is characterized by comprising the following components in percentage by weight: 10 to 60 percent of fluorine-containing water-based resin, 10 to 60 percent of fluorine-free water-based resin, 0.5 to 20 percent of auxiliary agent for water-based paint, 0 to 30 percent of film-forming auxiliary agent, 20 to 70 percent of deionized water and 0.4 to 3 percent of water-based closed isocyanate; the structure of the fluorine-containing water-based resin is shown as a formula I, and a silane coupling agent is copolymerized in the fluorine-free water-based resin
The preparation method of the fluorine-containing water-based resin comprises the following steps: the acrylate/fluorine-containing acrylate copolymer is prepared by mixing 4-25 wt% of acrylate monomer, 5-15 wt% of umbrella-shaped short-chain fluorine-containing compound monomer, surfactant, initiator and water.
2. The fluorine-containing aqueous self-layered coating according to claim 1, wherein the silane coupling agent is 0.1% to 2% by weight of the fluorine-free aqueous resin.
3. The fluorine-containing aqueous self-layered coating material according to claim 1, wherein the silane coupling agent monomer is at least one of γ -aminopropyltriethoxysilane, γ -glycidoxypropyltrimethoxysilane, and γ - (methacryloyloxy) propyltrimethoxysilane.
4. The fluorine-containing aqueous self-layered coating according to claim 1, wherein the fluorine-free aqueous resin is one or more of an aqueous polyacrylate resin, an aqueous polyurethane-polyacrylate composite resin, and an aqueous epoxy resin.
5. The fluorine-containing aqueous self-layered coating material according to claim 1, wherein the auxiliary agent for the aqueous coating material is a combination of one or more of a wetting agent, a dispersing agent, an antifoaming agent, a leveling agent, a thickening agent, a preservative and a mildewproofing agent.
6. The fluorine-containing aqueous self-layering coating of claim 1, wherein the coalescent is an organic solvent and the coalescent is miscible with water.
7. The fluorine-containing aqueous self-layering coating of claim 6, wherein the coalescent is one or a combination of propylene glycol butyl ether, propylene glycol methyl ether, dipropylene glycol methyl ether and dipropylene glycol butyl ether.
8. The method of preparing the fluorine-containing aqueous self-layered coating material according to claim 5, comprising the steps of:
adding part of water, a film-forming assistant and a defoaming agent into a mixing tank, and uniformly stirring; then adding fluorine-containing water-based resin and fluorine-free water-based resin, and uniformly stirring; then adding the flatting agent, the thickening agent, the preservative, the mildew preventive and the water-based closed isocyanate in sequence, and stirring uniformly; adjusting the viscosity and the pH value; filtering and discharging to obtain the fluorine-containing water-based self-layering coating.
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| CN114752240A (en) * | 2022-05-12 | 2022-07-15 | 深圳市漆优水漆科技有限公司 | Method for preparing fireproof, waterproof and antibacterial film |
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