CN109180983B - Long-acting antifogging and antifrosting film and preparation method thereof - Google Patents
Long-acting antifogging and antifrosting film and preparation method thereof Download PDFInfo
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/042—Coating with two or more layers, where at least one layer of a composition contains a polymer binder
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- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
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- C08J2327/00—Characterised by the use of 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 a halogen; Derivatives of such polymers
- C08J2327/02—Characterised by the use of 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 a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2327/04—Characterised by the use of 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 a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
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- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C08J2429/00—Characterised by the use of 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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08J2433/00—Characterised by the use of homopolymers or 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 of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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Abstract
The invention provides a long-acting antifogging and antifrosting film and a preparation method thereof, belonging to the technical field of high polymer materials. The film is formed by compounding a matrix polymer layer, an adhesive layer and a modified polyvinyl alcohol layer. The matrix polymer resin is polyethylene, polypropylene, polylactic acid, polyhydroxyalkanoate, polyvinyl chloride, polymethyl methacrylate, polystyrene, polycarbonate, polyamide, polyester, polyphenyl ether, polyurethane and polyacrylonitrile; the adhesive is water-based acrylic resin; the modified polyvinyl alcohol is prepared from a polyvinyl alcohol mixture, tetraethyl orthosilicate, an ethanol-water mixed solvent and a wetting agent. The invention has long-term antifogging and antifrosting, safety, no toxicity, low cost and easy realization of industrial production.
Description
Technical Field
The invention belongs to the technical field of high polymer materials, and particularly relates to a long-acting anti-fog and anti-frost film and a preparation method thereof.
Background
The production and use of transparent materials have penetrated in various aspects of people's life, but transparent materials such as glasses, face masks, bathroom glass, automobile front windshield, camera lenses and the like can fog or frost under certain environments, and the phenomenon brings much trouble to people, even causes great economic loss, so that the research on how to solve the antifogging and antifrosting problem of the transparent materials has great application value.
When the surface temperature of the transparent substrate is lower than the dew point of the surrounding water vapor, the saturated water vapor can be quenched and condensed into water drops to fall on the surface of the substrate, the light rays incident on the surface of the substrate are refracted and reflected through the water drops, the light transmittance of the transparent substrate is reduced, and the fog on the surface of the transparent substrate is formed under two conditions:
1) the temperature difference between the external environment and the surface of the substrate is as follows: when a certain amount of water vapor exists in the external environment and the temperature of the surface of the substrate is lower than the dew point of the water vapor in the environment, saturated water vapor can be quenched and form water drops;
2) in relation to the wettability of the substrate surface: the surface tension between the three phases solid, gas, liquid determines whether the substrate surface is atomized.
In recent years, researches on anti-fog and anti-frost materials by expert scholars can be mainly divided into two types, namely hydrophilic anti-fog and anti-frost materials and hydrophobic anti-fog and anti-frost materials. When the contact angle theta between the water drop and the surface of the base material is between 0 and 30 degrees, the water drop can completely soak and spread on the surface of the base material to form a uniform water film, so that the diffuse reflection of the dispersed water drop to light is eliminated, and the sight of people is not influenced. In this case, the surface of the transparent substrate can maintain optical transparency although condensation still occurs, and the water film formed on the surface is not seen at all when viewed in the vertical direction. The surface of a substrate in a hydrophobic state is less wettable or non-wettable to a liquid when the surface contact angle θ is greater than 90 °, and there are two main methods for constructing a hydrophobic surface: one approach is to construct regular coarse structures and to chemically modify these structures as necessary (Nature Materials,2017,16, 658-; another approach is to introduce low surface energy species and migrate low surface energy compounds to the surface of the substrate, and common low surface energy species mainly include fluorine (F), silicon (Si) containing compounds (ACS Applied Materials & Interfaces,2015,7(38),21021- & 21029). The hydrophobic antifogging material has small enough surface tension, water drops are easy to roll off and can not stay on the surface of the material, and the antifogging effect is achieved. In practical production application, hydrophobic antifogging materials are high in cost and cannot be widely applied, while hydrophilic antifogging materials are popular, but most materials cannot keep long-term effective antifogging and antifrosting effects due to special hydrophilicity.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a long-acting anti-fog and anti-frost film and a preparation method thereof. The material has long-term antifogging and antifrosting property, is safe and nontoxic, can be realized on the traditional simple synthesis equipment, has low cost and environmental protection, and is easy to realize industrial production.
The technical scheme of the invention is as follows:
the long-acting antifogging and antifrosting film is of a five-layer structure and sequentially comprises a modified polyvinyl alcohol layer, an adhesive layer, a matrix polymer layer, an adhesive layer and a modified polyvinyl alcohol layer.
The thickness of base member polymer layer is 5~600um, the thickness of modified polyvinyl alcohol layer is 0.5~50 um.
The resin used for the substrate polymer layer is made of polyethylene, polypropylene, polylactic acid, polyhydroxyalkanoate, polyvinyl chloride, polymethyl methacrylate, polystyrene, polycarbonate, polyamide, polyester, polyphenylene oxide, polyurethane or polyacrylonitrile.
The adhesive used in the adhesive layer is water-based acrylic resin.
The modified polyvinyl alcohol layer is prepared from a polyvinyl alcohol mixture, tetraethyl orthosilicate, an ethanol-water mixed solvent and a wetting agent, wherein the polyvinyl alcohol mixture is 3-12 parts by weight, the tetraethyl orthosilicate is 0.6-6 parts by weight and the wetting agent is 0.5-3 parts by weight based on 100 parts by weight of the ethanol-water mixed solvent.
The polyvinyl alcohol mixture comprises polyvinyl alcohol 1799, polyvinyl alcohol 1599 and polyvinyl alcohol 0599, wherein the polyvinyl alcohol 1599 accounts for 10-20 parts and the polyvinyl alcohol 0599 accounts for 5-10 parts by weight of 100 parts of the polyvinyl alcohol 1799.
The ethanol-water mixed solvent comprises 25-100 parts by weight of ethanol based on 100 parts by weight of water.
The wetting agent is acetylenic ethylene glycol, including 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol polyoxyethylene ether, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol polyoxyethylene polyoxypropylene ether, 2,5,8, 11-tetramethyl-6-dodecyne-5, 8-diol, 2,5,8, 11-tetramethyl-6-dodecene-5, 8-diol polyoxyethylene ether, 3, 5-dimethyl-1-hexyne-3-ol and 3, 6-dimethyl-1-heptyne-3-ol.
The preparation method of the long-acting antifogging and antifrosting film comprises the following steps: coating adhesive on two sides of the matrix polymer, drying, coating modified polyvinyl alcohol solution, drying and rolling.
The preparation method of the modified polyvinyl alcohol comprises the following steps:
(1) adding the polyvinyl alcohol mixture into an ethanol-water mixed solvent, heating to 95 ℃, and stirring until the polyvinyl alcohol mixture is completely dissolved;
(2) dripping HCl into the solution obtained in the step (1) to adjust the pH value to 2-3, dripping tetraethyl orthosilicate at normal temperature, and stirring;
(3) adding wetting agent and stirring evenly.
Compared with other antifogging and antifrosting materials, the basic idea of the method is to prepare the modified polyvinyl alcohol by tetraethyl orthosilicate hydrolytic crosslinking and add a specific wetting agent, so that the problems that the conventional common polyvinyl alcohol can not prevent fog and frost for a long time due to swelling in water, or an aldehyde crosslinking agent harmful to a body can not be completely soaked in a polymer film and the like are solved, the soaking performance of the modified polyvinyl alcohol coating liquid in a matrix polymer layer and an adhesive layer is improved, and the uniform composite film can be prepared.
The invention has the beneficial effects that: the multilayer composite film obtained by the preparation method provided by the invention has the characteristics of long-term antifogging property, long-term frost resistance, good wettability on polymer, safety, no toxicity and the like. The long-acting antifogging and antifrosting film can be realized on the traditional simple synthesis equipment, has low cost and environmental protection, and is easy to realize industrial production.
Detailed Description
The technical solution of the present invention will be further described with reference to specific examples.
Example 1
Weighing 2.6 parts of polyvinyl alcohol 1799, 0.26 part of polyvinyl alcohol 1599 and 0.14 part of polyvinyl alcohol 0599, adding a mixed solvent 1 of 80 parts of water and 20 parts of ethanol, heating to 95 ℃, and stirring until the mixture is completely dissolved; dropwise adding HCl, adjusting the pH value to 2-3, stirring for a period of time, dropwise adding 0.6 part of tetraethyl orthosilicate, stirring at normal temperature for reaction, and finally adding 0.5 part of 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol to prepare the modified polyvinyl alcohol solution 1.
Coating water-based polyacrylic resin (Tesmann Neocryl-A1127) on two sides of a polypropylene film with the thickness of 5um, completely drying, respectively coating the modified polyvinyl alcohol solution 1, and controlling the thickness of the dried modified polyvinyl alcohol layer to be 0.5um through the thickness of a coating device to prepare the antifogging and antifrosting film 1.
Example 2
Weighing 4 parts of polyvinyl alcohol 1799, 0.6 part of polyvinyl alcohol 1599 and 0.4 part of polyvinyl alcohol 0599, adding a mixed solvent 2 of 70 parts of water and 30 parts of ethanol, heating to 95 ℃, and stirring until the mixture is completely dissolved; dropwise adding HCl, adjusting the pH value to 2-3, stirring for a period of time, dropwise adding 2 parts of tetraethyl orthosilicate, stirring at normal temperature for reaction, and finally adding 1 part of 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol polyoxyethylene ether to prepare the modified polyvinyl alcohol solution 2.
Coating water-based polyacrylic resin (Tesman Neocryl A-1092) on both sides of a polyvinyl chloride film with the thickness of 50um, completely drying, respectively coating the modified polyvinyl alcohol solution 2, and controlling the thickness of the dried modified polyvinyl alcohol layer to be 10um by the thickness of a coating device to obtain the antifogging and antifrosting film 2.
Example 3
Weighing 8 parts of polyvinyl alcohol 1799, 1.6 parts of polyvinyl alcohol 1599 and 0.4 part of polyvinyl alcohol 0599, adding a mixed solvent 3 of 60 parts of water and 40 parts of ethanol, heating to 95 ℃, and stirring until the mixture is completely dissolved; dropwise adding HCl, adjusting the pH value to 2-3, dropwise adding 4 parts of tetraethyl orthosilicate after stirring for a period of time, stirring at normal temperature for reaction, and finally adding 1 part of 2,5,8, 11-tetramethyl-6-dodecyne-5, 8-diol and 1 part of 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol polyoxyethylene polyoxypropylene ether to prepare the modified polyvinyl alcohol solution 3.
Coating water-based polyacrylic resin (Tesman Neocryl A-1120) on both sides of a polycarbonate film with the thickness of 200um, completely drying, respectively coating the modified polyvinyl alcohol solution 3, and controlling the thickness of the dried modified polyvinyl alcohol layer to be 25um through the thickness of a coating device to prepare the antifogging and antifrosting film 3.
Example 4
Weighing 9.3 parts of polyvinyl alcohol 1799, 1.8 parts of polyvinyl alcohol 1599 and 0.9 part of polyvinyl alcohol 0599, adding a mixed solvent 4 of 50 parts of water and 50 parts of ethanol, heating to 95 ℃, and stirring until the mixture is completely dissolved; dropwise adding HCl, adjusting the pH value to 2-3, stirring for a period of time, dropwise adding 6 parts of tetraethyl orthosilicate, stirring at normal temperature for reaction, and finally adding 2 parts of 3, 5-dimethyl-1-hexyne-3-ol and 1 part of 2,5,8, 11-tetramethyl-6-dodecenyl-5, 8-diol polyoxyethylene ether to prepare the modified polyvinyl alcohol solution 4.
Coating water-based polyacrylic resin (Tesmann Neocryl XK-98) on two sides of a polyethylene terephthalate film with the thickness of 600um, completely drying, respectively coating the modified polyvinyl alcohol solution 4, and controlling the thickness of the dried modified polyvinyl alcohol layer to be 50um through the thickness of a coating device to prepare the antifogging and antifrosting film 4.
Comparative example 1
Weighing 10 parts of polyvinyl alcohol 1799, adding 100 parts of water, heating to 95 ℃, and stirring until the polyvinyl alcohol is completely dissolved to obtain the polyvinyl alcohol coating liquid.
The film 1 was prepared by coating a polypropylene film having a thickness of 5um on both sides with a water-based polyacrylic resin (Tesmann Neocryl-A1127), completely drying, coating the above polyvinyl alcohol solutions, respectively, and controlling the thickness of the dried polyvinyl alcohol layer to 0.5um by the thickness of the coater.
Comparative example 2
Weighing 10 parts of polyvinyl alcohol 1599, adding a mixed solvent of 70 parts of water and 30 parts of ethanol, heating to 95 ℃, and stirring until the polyvinyl alcohol is completely dissolved to obtain the polyvinyl alcohol coating liquid.
A polyvinyl chloride film having a thickness of 50 μm was coated on both sides with a water-based polyacrylic resin (Tesman Neocryl A-1092), and after completely drying, the polyvinyl alcohol solutions were coated, respectively, and the thickness of the dried polyvinyl alcohol layer was controlled to 10 μm by the thickness of the coater, to obtain film 2.
Comparative example 3
Weighing 8 parts of polyvinyl alcohol 1799, 1 part of polyvinyl alcohol 1599 and 1 part of polyvinyl alcohol 0599, adding a mixed solvent of 50 parts of water and 50 parts of ethanol, heating to 95 ℃, and stirring until the mixture is completely dissolved to obtain the polyvinyl alcohol coating liquid.
A polyethylene terephthalate film having a thickness of 600um was coated on both sides with a water-based polyacrylic resin (Tesmann Neocryl XK-98), and after completely drying, the above polyvinyl alcohol solutions were coated, respectively, and the thickness of the dried polyvinyl alcohol layer was controlled to 50um by the thickness of the coater, to obtain a film 3.
The films obtained in comparative examples 1 to 3 and examples 1 to 4 above were subjected to antifogging and antifrosting property tests, the test methods selected being as follows:
antifogging test: the test film was placed 5 mm above hot water at 80-100 c, the time was recorded, it was observed whether the film surface was hazy, and the water temperature was maintained during the test, the results are shown in table 1.
And (3) frost prevention test: the test film was placed in a refrigerator at-18 ℃ for 24 hours, taken out, and then observed whether the film surface was hazy and the time was recorded, and after 1 minute, the test was carried out at ambient temperature, and the haze was removed, the results are shown in table 2.
TABLE 1
TABLE 2
The composite film provided by the invention has long antifogging and antifrosting performance, good wettability on polymer, safety and innocuity, can be realized on traditional simple synthesis equipment, has low cost and environmental friendliness, and is easy to realize industrial production.
Those of ordinary skill in the art will understand that: the invention is not to be considered as limited to the specific embodiments thereof, but is to be understood as being modified in all respects, all changes and equivalents that come within the spirit and scope of the invention.
Claims (5)
1. The long-acting antifogging and antifrosting film is characterized by having a five-layer structure and sequentially comprising a modified polyvinyl alcohol layer, an adhesive layer, a matrix polymer layer, an adhesive layer and a modified polyvinyl alcohol layer;
the modified polyvinyl alcohol layer is prepared from a polyvinyl alcohol mixture, tetraethyl orthosilicate, an ethanol-water mixed solvent and a wetting agent, wherein the ethanol-water mixed solvent accounts for 100 parts by weight, the polyvinyl alcohol mixture accounts for 3-12 parts, the tetraethyl orthosilicate accounts for 0.6-6 parts, and the wetting agent accounts for 0.5-3 parts;
the polyvinyl alcohol mixture comprises polyvinyl alcohol 1799, polyvinyl alcohol 1599 and polyvinyl alcohol 0599, wherein the polyvinyl alcohol 1599 accounts for 10-20 parts and the polyvinyl alcohol 0599 accounts for 5-10 parts by weight of 100 parts of the polyvinyl alcohol 1799;
the thickness of the matrix polymer layer is 5-600 um, and the thickness of the modified polyvinyl alcohol layer is 0.5-50 um;
the preparation method of the long-acting antifogging and antifrosting film comprises the following steps: (1) adding the polyvinyl alcohol mixture into an ethanol-water mixed solvent, heating to 95 ℃, and stirring until the polyvinyl alcohol mixture is completely dissolved; (2) dripping HCl into the solution obtained in the step (1) to adjust the pH value to 2-3, dripping tetraethyl orthosilicate at normal temperature, and stirring; (3) adding wetting agent and stirring evenly.
2. The long-acting antifogging and antifrosting film according to claim 1, wherein the wetting agent is an acetylenic glycol comprising 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol polyoxyethylene ether, 2,4,7, 9-tetramethyl-5-decyne-4, 7-diol polyoxyethylene polyoxypropylene ether, 2,5,8, 11-tetramethyl-6-dodecene-5, 8-diol polyoxyethylene ether, 3, 5-dimethyl-1-hexyn-3-ol, One or more than two of 3, 6-dimethyl-1-heptyne-3-ol are mixed.
3. The long-acting antifogging and antifrosting film according to claim 1, wherein the ethanol-water mixed solvent is 25 to 100 parts by weight of ethanol based on 100 parts by weight of water.
4. The long-acting antifog and antifrost film according to claim 1, 2 or 3, wherein the base polymer layer is prepared from polyethylene, polypropylene, polylactic acid, polyhydroxyalkanoate, polyvinyl chloride, polymethyl methacrylate, polystyrene, polycarbonate, polyamide, polyester, polyphenylene oxide, polyurethane or polyacrylonitrile; the adhesive used in the adhesive layer is water-based acrylic resin.
5. A method for preparing the long-acting antifogging and antifrosting film as claimed in any one of claims 1 to 4, characterized in that the adhesive is coated on both sides of the matrix polymer, after drying, the modified polyvinyl alcohol solution is coated respectively, and then drying and rolling are carried out.
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|---|---|---|---|---|
| GB1314827A (en) * | 1969-08-07 | 1973-04-26 | Agfa Gevaert | Prevention of mist formation on transparent sheet material |
| CN1158881A (en) * | 1995-10-27 | 1997-09-10 | 住友化学工业株式会社 | Antifog film |
| CN1442463A (en) * | 2003-04-04 | 2003-09-17 | 四川大学 | Agricultural long effect antimist film and its preparation method |
| CN105368188A (en) * | 2014-09-01 | 2016-03-02 | 中国科学院理化技术研究所 | Preparation method of water-resistant long-acting anti-fog and anti-frost coating with controllable crosslinking degree |
| CN106833169A (en) * | 2017-01-12 | 2017-06-13 | 和智创成（北京）科技有限公司 | The preparation method and application of the long-acting antifog clear coat of high intensity |
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2018
- 2018-09-25 CN CN201811118536.8A patent/CN109180983B/en active Active
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|---|---|---|---|---|
| GB1314827A (en) * | 1969-08-07 | 1973-04-26 | Agfa Gevaert | Prevention of mist formation on transparent sheet material |
| CN1158881A (en) * | 1995-10-27 | 1997-09-10 | 住友化学工业株式会社 | Antifog film |
| CN1442463A (en) * | 2003-04-04 | 2003-09-17 | 四川大学 | Agricultural long effect antimist film and its preparation method |
| CN105368188A (en) * | 2014-09-01 | 2016-03-02 | 中国科学院理化技术研究所 | Preparation method of water-resistant long-acting anti-fog and anti-frost coating with controllable crosslinking degree |
| CN106833169A (en) * | 2017-01-12 | 2017-06-13 | 和智创成（北京）科技有限公司 | The preparation method and application of the long-acting antifog clear coat of high intensity |
Non-Patent Citations (1)
| Title |
|---|
| "溶胶-凝胶法制备PVA/SiO2杂化材料及性能表征";李人哲等;《涂料工业》;20060401;第36卷(第04期);第21-27页 * |
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