CN111876044A - Coating liquid for long-term antifogging film and preparation method thereof - Google Patents
Coating liquid for long-term antifogging film and preparation method thereof Download PDFInfo
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- CN111876044A CN111876044A CN202010673682.8A CN202010673682A CN111876044A CN 111876044 A CN111876044 A CN 111876044A CN 202010673682 A CN202010673682 A CN 202010673682A CN 111876044 A CN111876044 A CN 111876044A
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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
- C09D133/14—Homopolymers or copolymers of esters of esters containing halogen, nitrogen, sulfur or oxygen atoms in addition to the carboxy oxygen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- 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
- C08F220/20—Esters of polyhydric alcohols or phenols, e.g. 2-hydroxyethyl (meth)acrylate or glycerol mono-(meth)acrylate
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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
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The invention discloses a coating liquid for a long-term antifogging film and a preparation method thereof, wherein the coating liquid comprises the following substances in percentage by mass: 7-12% of aqueous polyurethane emulsion, 5-10% of polyvinyl alcohol, 8-15% of hydrophilic acrylic resin, 0.5-1.5% of nano silicon dioxide, 0.2-1% of silane coupling agent, 0.5-1.5% of surfactant and the like. The coating liquid can be directly coated on the surface of the film, is cured by UV, has the advantages of high adhesion strength with the film, good durability, washing resistance and wiping resistance, good hydrophilicity, excellent antifogging property and good oxygen barrier property, can effectively prolong the aging and yellowing time of the film, and has good use effect.
Description
Technical Field
The invention relates to the field of film production, in particular to a coating liquid of a long-term antifogging film and a preparation method thereof.
Background
The atomization and the condensation of the transparent film material are common problems in production and life, and cause great trouble to people. For example, a solar cell thin film, the energy utilization rate of a solar cell is proportional to the transmittance of light, and obviously, fogging may reduce the energy utilization rate. For example, the application of packaging film, food package or electronic device package, etc. can directly affect the quality reliability of food or electronic device. The main methods for solving such problems are physical heating defogging, hydrophilic or hydrophobic coating antifogging. The traditional thermosetting film forming method at present has the defects of high energy consumption, low efficiency, easy deformation of a base material and the like. The traditional mode of coating the antifogging coating liquid on the surface of the film to form a coating has the problems of unsatisfactory antifogging effect, poor durability and easy failure.
Disclosure of Invention
In order to solve the technical problems, the invention provides a coating liquid for a long-term antifogging film and a preparation method thereof, which solve the problems of unsatisfactory antifogging effect, poor durability and easy failure of the traditional mode of coating the antifogging coating liquid on the surface of the film to form a coating by compounding the aqueous polyurethane emulsion, the polyvinyl alcohol and the hydrophilic acrylic resin and matching with other auxiliaries.
In order to achieve the purpose, the technical scheme of the invention is as follows: a coating liquid for a long-lasting antifogging film comprises the following substances in percentage by mass:
in a preferred embodiment of the present invention, the hydrophilic acrylic resin is prepared from hydroxyethyl acrylate, methyl acrylate, glycidyl methacrylate, chain transfer agent DDMAT, photoinitiator TPO, and chloroform.
In a preferred embodiment of the present invention, the silane coupling agent is one or a mixture of two or more of vinyltriethoxysilane, gamma-aminopropyltriethoxysilane and vinyltrimethoxysilane.
In a preferred embodiment of the present invention, the surfactant is T-80.
In a preferable embodiment of the present invention, the particle size of the nano-silica is 1 to 500 nm.
In a preferred embodiment of the present invention, the coating thickness of the coating liquid after drying and photocuring is 1.2 to 5 μm.
The preparation method of the coating liquid for the long-term antifogging film comprises the following steps:
step 1, preparing hydrophilic acrylic resin; sequentially adding 30mol of hydroxyethyl acrylate, 20mol of methyl acrylate, 5mol of glycidyl methacrylate, 0.5mol of chain transfer agent DDMAT, 0.02mol of photoinitiator TPO and 2.5mol of newly steamed chloroform into a reaction vessel, shading by using a black film, stirring in a sealed way, and introducing nitrogen to discharge oxygen; placing the reaction container under an ultraviolet lamp, and carrying out polymerization reaction at 25 ℃ under the protection of nitrogen by using long-wave ultraviolet visible radiation as an activation source for 3 hours; precipitating a polymerization product obtained by the reaction with anhydrous ether, drying in a vacuum drying oven for 24 hours, and sealing and storing to obtain hydrophilic acrylic resin;
step 2, preparing a coating liquid; preparing raw materials according to a proportion, adding the aqueous polyurethane emulsion, polyvinyl alcohol and hydrophilic acrylic resin into absolute ethyl alcohol, mixing and stirring, and adding distilled water to prepare a mixed solution; adding a silane coupling agent into the nano silicon dioxide dispersion liquid, reacting at 50-80 ℃ for 0.5-1h, and adding into the mixed solution; and stirring the mixed solution surfactant and the viscosity regulator for 1-2h to form a coating liquid.
As a preferable embodiment of the above preparation method, the method further comprises step 3 of toning the coating liquid; the coating liquid was irradiated with ultraviolet rays until the coating liquid became colorless.
Through the technical scheme, the technical scheme of the invention has the following remarkable beneficial effects: the coating liquid can be directly coated on the surface of the film, is cured by UV, has the advantages of high adhesion strength with the film, good durability, washing resistance and wiping resistance, good hydrophilicity, excellent antifogging property and good oxygen barrier property, can effectively prolong the aging and yellowing time of the film, and has good use effect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 raw material sources are as follows:
example 1
A coating liquid for a long-lasting antifogging film comprises the following substances in percentage by mass:
the hydrophilic acrylic resin is prepared from hydroxyethyl acrylate, methyl acrylate, glycidyl methacrylate, a chain transfer agent DDMAT, a photoinitiator TPO and chloroform. The silane coupling agent is one or more of vinyl triethoxysilane, gamma-aminopropyl triethoxysilane, and vinyl trimethoxysilane. The surfactant is a surfactant T-80. The particle size of the nano silicon dioxide is 1-500 nm. The coating thickness formed after the coating liquid is dried and cured is 2.1 mu m.
The preparation method of the coating liquid for the long-term antifogging film comprises the following steps:
step 1, preparing hydrophilic acrylic resin; sequentially adding 30mol of hydroxyethyl acrylate, 20mol of methyl acrylate, 5mol of glycidyl methacrylate, 0.5mol of chain transfer agent DDMAT, 0.02mol of photoinitiator TPO and 2.5mol of newly steamed chloroform into a reaction vessel, shading by using a black film, stirring in a sealed way, and introducing nitrogen to discharge oxygen; placing the reaction container under an ultraviolet lamp, and carrying out polymerization reaction at 25 ℃ under the protection of nitrogen by using long-wave ultraviolet visible radiation as an activation source for 3 hours; and (3) settling a polymerization product obtained by the reaction with anhydrous ether, drying in a vacuum drying oven for 24 hours, and sealing and storing to obtain the hydrophilic acrylic resin.
Step 2, preparing a coating liquid; preparing raw materials according to a proportion, adding the aqueous polyurethane emulsion, polyvinyl alcohol and hydrophilic acrylic resin into absolute ethyl alcohol, mixing and stirring, and adding distilled water to prepare a mixed solution; adding a silane coupling agent into the nano silicon dioxide dispersion liquid, reacting at 50-80 ℃ for 0.5-1h, and adding into the mixed solution; and stirring the mixed solution surfactant and the viscosity regulator for 1-2h to form a coating liquid.
Step 3, toning the coating liquid; the coating liquid was irradiated with ultraviolet rays until the coating liquid became colorless.
Example 2
A coating liquid for a long-lasting antifogging film comprises the following substances in percentage by mass:
the hydrophilic acrylic resin is prepared from hydroxyethyl acrylate, methyl acrylate, glycidyl methacrylate, a chain transfer agent DDMAT, a photoinitiator TPO and chloroform. The silane coupling agent is one or more of vinyl triethoxysilane, gamma-aminopropyl triethoxysilane, and vinyl trimethoxysilane. The surfactant is a surfactant T-80. The particle size of the nano silicon dioxide is 1-500 nm. The coating thickness formed after the coating liquid was dried and cured was 1.6 μm. .
The preparation method of the coating liquid for the long-term antifogging film comprises the following steps:
step 1, preparing hydrophilic acrylic resin; sequentially adding 30mol of hydroxyethyl acrylate, 20mol of methyl acrylate, 5mol of glycidyl methacrylate, 0.5mol of chain transfer agent DDMAT, 0.02mol of photoinitiator TPO and 2.5mol of newly steamed chloroform into a reaction vessel, shading by using a black film, stirring in a sealed way, and introducing nitrogen to discharge oxygen; placing the reaction container under an ultraviolet lamp, and carrying out polymerization reaction at 25 ℃ under the protection of nitrogen by using long-wave ultraviolet visible radiation as an activation source for 3 hours; and (3) settling a polymerization product obtained by the reaction with anhydrous ether, drying in a vacuum drying oven for 24 hours, and sealing and storing to obtain the hydrophilic acrylic resin.
Step 2, preparing a coating liquid; preparing raw materials according to a proportion, adding the aqueous polyurethane emulsion, polyvinyl alcohol and hydrophilic acrylic resin into absolute ethyl alcohol, mixing and stirring, and adding distilled water to prepare a mixed solution; adding a silane coupling agent into the nano silicon dioxide dispersion liquid, reacting at 50-80 ℃ for 0.5-1h, and adding into the mixed solution; and stirring the mixed solution surfactant and the viscosity regulator for 1-2h to form a coating liquid.
Example 3
A coating liquid for a long-lasting antifogging film comprises the following substances in percentage by mass:
the hydrophilic acrylic resin is prepared from hydroxyethyl acrylate, methyl acrylate, glycidyl methacrylate, a chain transfer agent DDMAT, a photoinitiator TPO and chloroform. The silane coupling agent is one or more of vinyl triethoxysilane, gamma-aminopropyl triethoxysilane, and vinyl trimethoxysilane. The surfactant is a surfactant T-80. The particle size of the nano silicon dioxide is 1-500 nm. The coating thickness formed after the coating liquid is dried and cured is 2.8 mu m.
The preparation method of the coating liquid for the long-term antifogging film comprises the following steps:
step 1, preparing hydrophilic acrylic resin; sequentially adding 30mol of hydroxyethyl acrylate, 20mol of methyl acrylate, 5mol of glycidyl methacrylate, 0.5mol of chain transfer agent DDMAT, 0.02mol of photoinitiator TPO and 2.5mol of newly steamed chloroform into a reaction vessel, shading by using a black film, stirring in a sealed way, and introducing nitrogen to discharge oxygen; placing the reaction container under an ultraviolet lamp, and carrying out polymerization reaction at 25 ℃ under the protection of nitrogen by using long-wave ultraviolet visible radiation as an activation source for 3 hours; precipitating a polymerization product obtained by the reaction with anhydrous ether, drying in a vacuum drying oven for 24 hours, and sealing and storing to obtain hydrophilic acrylic resin;
step 2, preparing a coating liquid; preparing raw materials according to a proportion, adding the aqueous polyurethane emulsion, polyvinyl alcohol and hydrophilic acrylic resin into absolute ethyl alcohol, mixing and stirring, and adding distilled water to prepare a mixed solution; adding a silane coupling agent into the nano silicon dioxide dispersion liquid, reacting at 50-80 ℃ for 0.5-1h, and adding into the mixed solution; and stirring the mixed solution surfactant and the viscosity regulator for 1-2h to form a coating liquid.
Step 3, toning the coating liquid; the coating liquid was irradiated with ultraviolet rays until the coating liquid became colorless.
Example 4
A coating liquid for a long-lasting antifogging film comprises the following substances in percentage by mass:
the hydrophilic acrylic resin is prepared from hydroxyethyl acrylate, methyl acrylate, glycidyl methacrylate, a chain transfer agent DDMAT, a photoinitiator TPO and chloroform. The silane coupling agent is one or more of vinyl triethoxysilane, gamma-aminopropyl triethoxysilane, and vinyl trimethoxysilane. The surfactant is a surfactant T-80. The particle size of the nano silicon dioxide is 1-500 nm. The coating thickness formed after the coating liquid was dried and cured was 2.6 μm.
The preparation method of the coating liquid for the long-term antifogging film comprises the following steps:
step 1, preparing hydrophilic acrylic resin; sequentially adding 30mol of hydroxyethyl acrylate, 20mol of methyl acrylate, 5mol of glycidyl methacrylate, 0.5mol of chain transfer agent DDMAT, 0.02mol of photoinitiator TPO and 2.5mol of newly steamed chloroform into a reaction vessel, shading by using a black film, stirring in a sealed way, and introducing nitrogen to discharge oxygen; placing the reaction container under an ultraviolet lamp, and carrying out polymerization reaction at 25 ℃ under the protection of nitrogen by using long-wave ultraviolet visible radiation as an activation source for 3 hours; precipitating a polymerization product obtained by the reaction with anhydrous ether, drying in a vacuum drying oven for 24 hours, and sealing and storing to obtain hydrophilic acrylic resin;
step 2, preparing a coating liquid; preparing raw materials according to a proportion, adding the aqueous polyurethane emulsion, polyvinyl alcohol and hydrophilic acrylic resin into absolute ethyl alcohol, mixing and stirring, and adding distilled water to prepare a mixed solution; adding a silane coupling agent into the nano silicon dioxide dispersion liquid, reacting at 50-80 ℃ for 0.5-1h, and adding into the mixed solution; and stirring the mixed solution surfactant and the viscosity regulator for 1-2h to form a coating liquid.
Step 3, toning the coating liquid; the coating liquid was irradiated with ultraviolet rays until the coating liquid became colorless.
The coating liquids of examples 1 to 4 were respectively coated on the surface of a PVC film having a thickness of 0.8mm by a doctor blade method, air-dried for 10min, cured for 1 min under a UV light of 600. mu.W, and then dried in a vacuum drying oven at 70 ℃ to form an antifogging coating on the PVC film.
Adhesion test
The adhesion between the coating layer of the composite film and the PVC film as the substrate is tested according to the GB 9286-1998 standard, the results of the examples 1 and 2 are difficult to peel, and the structures of the examples 3 and 4 are difficult to peel.
Testing of antifogging Properties
Antifogging time: the PVC films corresponding to examples 1 to 4 were placed on a resin frame so that the surface to be inspected faced downward at an inclination of 15 degrees to the horizontal plane. The resin frame was placed in saturated water vapor at 55 ℃ and a timer was started to measure the time at which fogging of the coating surface started. The experiment was repeated five times and the average was taken. Examples 1 to 4 showed no fogging phenomenon within 60 seconds, and exhibited excellent antifogging property.
Water resistance test
The PVC films corresponding to examples 1 to 4 were immersed in distilled water under ambient conditions, so that the surface of the coating appeared whitish or cracked and peeled. The length of time is used to characterize the water resistance of the coating film. None of examples 1-4 showed significant whitening or splitting after 3h soaking.
Oxygen permeability test
The prepared composite film was subjected to an oxygen transmission rate test using a Labthink VAC-V2 type pressure difference method gas permeameter, and the oxygen transmission rates of examples 1 to 4 were 3.4cm respectively3/m2·24h·0.1MPa、3.8cm3/m2·24h·0.1MPa、2.4cm3/m2·24h·0.1MPa、2.7cm3/m2·24h·0.1MPa。
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The coating liquid for the long-term antifogging film is characterized by comprising the following substances in percentage by mass:
2. the coating solution for a long-lasting antifogging film according to claim 1, wherein said hydrophilic acrylic resin is prepared from hydroxyethyl acrylate, methyl acrylate, glycidyl methacrylate, chain transfer agent DDMAT, photoinitiator TPO and chloroform.
3. The coating liquid for long-lasting antifogging film according to claim 2, wherein said silane coupling agent is one or a mixture of two or more of vinyltriethoxysilane, gamma-aminopropyltriethoxysilane, and vinyltrimethoxysilane.
4. The coating liquid for long-lasting antifogging film according to claim 2, wherein said surfactant is surfactant T-80.
5. The coating liquid for long-lasting antifogging film according to claim 2, wherein the nano silica has a particle size of 1 to 500 nm.
6. The coating liquid for a long-lasting antifogging film according to claim 2, wherein the coating layer has a thickness of 1.2-5 μm after drying and photocuring.
7. A method for preparing a coating liquid for a long-lasting antifogging film according to any one of claims 1 to 6, comprising the steps of:
step 1, preparing hydrophilic acrylic resin; sequentially adding 30mol of hydroxyethyl acrylate, 20mol of methyl acrylate, 5mol of glycidyl methacrylate, 0.5mol of chain transfer agent DDMAT, 0.02mol of photoinitiator TPO and 2.5mol of newly steamed chloroform into a reaction vessel, shading by using a black film, stirring in a sealed way, and introducing nitrogen to discharge oxygen; placing the reaction container under an ultraviolet lamp, and carrying out polymerization reaction at 25 ℃ under the protection of nitrogen by using long-wave ultraviolet visible radiation as an activation source for 3 hours; precipitating a polymerization product obtained by the reaction with anhydrous ether, drying in a vacuum drying oven for 24 hours, and sealing and storing to obtain hydrophilic acrylic resin;
step 2, preparing a coating liquid; preparing raw materials according to a proportion, adding the aqueous polyurethane emulsion, polyvinyl alcohol and hydrophilic acrylic resin into absolute ethyl alcohol, mixing and stirring, and adding distilled water to prepare a mixed solution; adding a silane coupling agent into the nano silicon dioxide dispersion liquid, reacting at 50-80 ℃ for 0.5-1h, and adding into the mixed solution; and stirring the mixed solution surfactant and the viscosity regulator for 1-2h to form a coating liquid.
8. The method for preparing the coating liquid for a long-lasting antifogging film according to claim 7, further comprising step 3 of toning the coating liquid; the coating liquid was irradiated with ultraviolet rays until the coating liquid became colorless.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113583529A (en) * | 2021-08-09 | 2021-11-02 | 海南必凯水性新材料有限公司 | Aqueous coating liquid, preparation method thereof and application of aqueous coating liquid in UV ink printing |
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| CN101649171A (en) * | 2009-08-31 | 2010-02-17 | 广东达美胶粘制品有限公司 | Solvent-free ultraviolet curing pressure sensitive adhersive for polyethylene protective film and preparation method thereof |
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Application publication date: 20201103 |