CN112940324A - Preparation method of efficient water-absorbing antifogging agricultural PET composite film - Google Patents
Preparation method of efficient water-absorbing antifogging agricultural PET composite film Download PDFInfo
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Abstract
The invention discloses aA preparation method of an efficient water-absorbing antifogging agricultural PET composite film is characterized in that the PET composite film is of a three-layer structure, a corona PET biaxial stretching film is used as a matrix, a modified cellulose high-water-absorption coating is coated on the surface of the matrix as a water-absorbing layer, and then a PVA @ SiO layer is coated on the surface of the matrix2The coating is a hydrophilic protective layer, wherein the base material of the modified cellulose is natural cellulose or carboxymethyl cellulose, and the monomer is a hydrophilic monomer comprising (methyl) acrylic acid, acrylamide, acrylonitrile, sodium p-styrene sulfonate and 2-acrylamide-2-methylpropanesulfonic acid. The PET composite film prepared by the invention has good weather resistance, can be used for a long time at low temperature, and is PVA @ SiO2The coating is wear-resistant and antistatic, has high water vapor permeability, can transfer fog to the modified cellulose high-water-absorption coating for absorption, realizes high-efficiency fog prevention, and has important significance for agricultural production.
Description
Technical Field
The invention relates to the technical field of agricultural antifogging, in particular to a preparation method of an agricultural PET composite film with high-efficiency water absorption and antifogging effects.
Background
The traditional PE and PVC agricultural films have high light transmittance and low price, but the weather resistance and mechanical property of the existing agricultural films are deteriorated due to large temperature difference change in severe cold areas and winter, the fog drop prevention function is lost, the light transmittance is reduced, the growth of crops is influenced, and the use time is greatly shortened, so that the use of the agricultural films is severely limited. Meanwhile, along with the gradual depletion of petroleum resources, the problem of environmental pollution is brought to attention of people, and the problem of white pollution of agricultural film products such as polyethylene and polyvinyl chloride to cultivated land is also urgently needed to be solved by research and development of novel green recyclable agricultural film products.
The biaxially oriented PET film has high strength, good transparency and good weather resistance, can be used at low temperature for a long time, is environment-friendly, pollution-free, recyclable and is the preferred film for agricultural use, but the PET film is easy to fog and is the problem to be solved for the first time as an agricultural film for preventing fog drops.
Disclosure of Invention
The invention aims to provide a preparation method of an efficient water-absorbing antifogging agricultural PET composite film, and aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a process for preparing the efficient water-absorbing antifogging agricultural PET composite film includes such steps as coating a high-hydroscopicity cellulose coating on the corona-treated bidirectional PET film, and coating a PVA @ SiO layer2The hydrophilic coating forms a three-layer composite membrane structure, and is characterized by comprising the following steps:
step one, preparing a cellulose-based high-water-absorption casting solution, which comprises the following steps:
dissolving a certain amount of natural cellulose or carboxymethyl cellulose, adding monomers in proportion, stirring in a constant-temperature stirrer, heating the temperature to a specified temperature, adding a certain amount of initiator, carrying out the whole reaction under the protection of nitrogen, cooling the reaction temperature to room temperature after reacting for a period of time, adding a cross-linking agent N, N' -methylene bisacrylamide, stirring for 30 minutes at room temperature, adding a proper amount of distilled water to adjust to a proper viscosity, and stopping stirring, standing and defoaming for later use;
step two, preparing the cellulose high water absorption coating, which comprises the following steps:
fixing the cleaned PET biaxially oriented film on a heating table, extruding the casting solution prepared in the step one on one end of the PET biaxially oriented film, quickly and uniformly coating the casting solution on the surface of the PET biaxially oriented film by using a scraper, pre-evaporating for 10 seconds at a preset temperature, quickly transferring the coated PET biaxially oriented film into a vacuum oven for heating and crosslinking, soaking the film in ethanol after crosslinking is completed, taking out the film and drying the film by using nitrogen for later use;
step three, PVA @ SiO2The preparation of the hydrophilic coating is as follows:
dissolving PVA in distilled water, adding hydrophilic silicon dioxide, dispersing uniformly, standing for defoaming, fixing the PET biaxial stretching film coated with the cellulose super-absorbent coating prepared in the step two on a heating table, and fixing the PVA @ SiO2The solution is uniformly coated on the surface of the PET biaxial stretching film by a scraper at a certain temperature, and then the PET biaxial stretching film is placed in an oven at 80 ℃ for drying to obtain the high-efficiency water-absorbing antifogging agricultural PET composite film.
Furthermore, the cellulose used in the cellulose-based super-absorbent membrane casting solution is natural cellulose and carboxymethyl cellulose, and the concentration of the cellulose is 0.2-8 wt%.
Further, the cellulose-based super-absorbent membrane casting solution adopts an aqueous solution polymerization method.
Furthermore, the cellulose-based super-absorbent casting solution adopts any one or more of (meth) acrylic acid, acrylamide, acrylonitrile, sodium p-styrenesulfonate and 2-acrylamide-2-methylpropanesulfonic acid as monomers which are added in any proportion.
Further, the reaction temperature of the cellulose-based super-absorbent membrane casting solution is 55-80 ℃, and the reaction time is 1-10 hours.
Furthermore, the addition amount of the initiator of the cellulose-based super-absorbent casting solution is 0.5-50% of the mass of the cellulose, and the addition amount of the cross-linking agent N, N' -methylene bisacrylamide is 0.5-50%.
Further, the crosslinking temperature of the cellulose-based super absorbent coating is 50-150 ℃, and the crosslinking time is 0.5-24 hours.
Further, the pre-evaporation temperature of the cellulose-based super absorbent coating is 30-150 ℃ during coating.
Further, the PVA @ SiO2The mass concentration of PVA in the hydrophilic coating is 3-20 wt%, and the water-based SiO is2The mass concentration of (A) is 0.01 wt% -15 wt%.
Further, PVA @ SiO in the third step2The coating temperature of the hydrophilic coating is 25-150 ℃.
Compared with the prior art, the invention has the following beneficial effects: the PET composite film prepared by the invention has good weather resistance, can be used for a long time at low temperature, and is PVA @ SiO2The coating is wear-resistant and antistatic, has high water vapor permeability, can transfer fog to the modified cellulose high-water-absorption coating for absorption, realizes efficient fog prevention, uses an industrialized film surface coating process, is simple to operate, wide in raw material source, low in price, environment-friendly, pollution-free and recyclable, high in light transmittance of the composite film, obvious in fog prevention effect, not easy to lose efficacy, and capable of being used at low temperature for a long time, and has important significance for agricultural production.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings needed in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings without creative efforts.
FIG. 1 is a schematic structural view of a PET composite film according to the present invention;
FIG. 2 is a contact angle diagram of the high-efficiency water-absorbing antifogging agricultural PET composite film prepared in example 1.
FIG. 3 is a test chart of antifogging performance of the high efficiency water absorption antifogging agricultural PET composite film prepared in example 1.
FIG. 4 is a graph of the light transmittance of each product of example 1.
Reference numerals:
1. a PET biaxially oriented film; 2. a cellulosic superabsorbent coating; 3. PVA @ SiO2A hydrophilic coating.
Detailed Description
The invention will be further described with reference to specific embodiments:
example 1
(1) Preparation of cellulose-based high-water-absorption casting solution
Dissolving 0.2g of cellulose in 7% NaOH/12% urea aqueous solution, adding 1g of acrylamide, starting stirring, heating the temperature to 60 ℃, stirring for 1 hour, adding 2g of acrylic acid and 0.012g of potassium persulfate, carrying out the whole reaction under the protection of nitrogen, cooling the reaction temperature to room temperature after 2 hours of reaction, adding 0.007g of cross-linking agent N, N' -methylene bisacrylamide, stirring for 30 minutes at room temperature, adding distilled water to adjust to proper viscosity, stopping stirring, standing and defoaming for later use.
(2) Preparation of cellulose superabsorbent coating 2
Fixing the cleaned PET biaxially oriented film 1 on a heating table, extruding the casting solution prepared in the step (1) at one end of the PET biaxially oriented film 1, quickly and uniformly coating the casting solution on the surface of the PET biaxially oriented film 1 by using a scraper, pre-evaporating at 50 ℃ for 10 seconds, quickly transferring the coated PET biaxially oriented film 1 into a vacuum oven, heating and crosslinking at 60 ℃ for 4 hours, soaking in ethanol after crosslinking is completed, taking out, and drying by using nitrogen for later use.
(3)PVA@SiO2Preparation of hydrophilic coating 3
Preparation of 11wt% of PVA aqueous solution, adding 0.05 wt% of hydrophilic silica, uniformly dispersing, standing for defoaming, fixing a PET biaxial stretching film on a heating table, and fixing PVA @ SiO2The solution is evenly coated on the surface of the PET biaxial stretching film 1 by a scraper at 100 ℃, and then the PET biaxial stretching film is placed in an oven at 80 ℃ for drying.
Example 2
(1) Preparation of cellulose-based high-water-absorption casting solution
Dissolving 0.2g of carboxymethyl cellulose in 9.8g of distilled water, adding 2g of acrylic acid with the neutralization degree of 75% and 0.040g of potassium persulfate, starting stirring, heating to 60 ℃, carrying out the whole reaction under the protection of nitrogen, reducing the reaction temperature to room temperature after reacting for 3 hours, adding 0.010g of cross-linking agent N, N' -methylene bisacrylamide, stirring for 30 minutes at room temperature, adding distilled water to adjust to a proper viscosity, stopping stirring, standing and defoaming for later use.
(2) Preparation of cellulose superabsorbent coating 2
Fixing the cleaned PET biaxially oriented film 1 on a heating table, extruding the casting solution prepared in the step (1) at one end of the PET biaxially oriented film 1, quickly and uniformly coating the casting solution on the surface of the PET biaxially oriented film 1 by using a scraper, pre-evaporating at 50 ℃ for 10 seconds, quickly transferring the coated PET biaxially oriented film 1 into a vacuum oven, heating and crosslinking at 60 ℃ for 4 hours, soaking in ethanol after crosslinking is completed, taking out, and drying by using nitrogen for later use.
(3)PVA@SiO2Preparation of hydrophilic coating 3
Preparing 11 wt% PVA aqueous solution, adding 0.05 wt% hydrophilic silica, uniformly dispersing, standing for defoaming, fixing the PET biaxial stretching film 1 on a heating table, and fixing the PVA @ SiO2The solution is uniformly coated on the surface of the PET biaxial stretching film 1 by a scraper at 100 ℃, and then the PET biaxial stretching film is placed in an oven at 80 ℃ for drying to obtain the PET composite film.
Example 3
(1) Preparation of cellulose-based high-water-absorption casting solution
Dissolving 0.2g of cellulose in 7% NaOH/12% urea aqueous solution, adding 0.5g of acrylamide, starting stirring, heating the temperature to 65 ℃, stirring for 1 hour, adding 2g of acrylic acid and 0.012g of potassium persulfate, carrying out the whole reaction under the protection of nitrogen, cooling the reaction temperature to room temperature after 2 hours of reaction, adding 0.005g of cross-linking agent N, N' -methylenebisacrylamide, stirring for 30 minutes at room temperature, adding distilled water to adjust to proper viscosity, stopping stirring, standing and defoaming for later use.
(2) Preparation of cellulose superabsorbent coating 2
Fixing the cleaned PET biaxially oriented film 1 on a heating table, extruding the casting solution prepared in the step (1) at one end of the PET biaxially oriented film 1, quickly and uniformly coating the casting solution on the surface of the PET biaxially oriented film 1 by using a scraper, pre-evaporating at 50 ℃ for 10 seconds, quickly transferring the coated PET biaxially oriented film 1 into a vacuum oven, heating and crosslinking at 70 ℃ for 4 hours, soaking in ethanol after crosslinking is completed, taking out, and drying by using nitrogen for later use.
(3)PVA@SiO2Preparation of hydrophilic coating 3
Preparing 5 wt% PVA aqueous solution, adding 0.05 wt% hydrophilic silica, dispersing uniformly, standing for defoaming, fixing a PET biaxial stretching film on a heating table, and fixing PVA @ SiO2The solution is evenly coated on the surface of the PET biaxial stretching film 1 by a scraper at 100 ℃, and then the PET biaxial stretching film is placed in an oven at 80 ℃ for drying.
Example 4
(1) Preparation of cellulose-based high-water-absorption casting solution
Dissolving 0.2g of carboxymethyl cellulose in 9.8g of distilled water, adding 2g of acrylic acid with 75% of neutralization degree and 0.0400g of potassium persulfate, starting stirring, heating to 60 ℃, carrying out the whole reaction under the protection of nitrogen, cooling the reaction temperature to room temperature after 3 hours of reaction, adding 0.008g of cross-linking agent N, N' -methylenebisacrylamide, stirring for 60 minutes at room temperature, adding distilled water to adjust to proper viscosity, stopping stirring, standing and defoaming for later use.
(2) Preparation of cellulose superabsorbent coating 2
Fixing the cleaned PET biaxially oriented film 1 on a heating table, extruding the casting solution prepared in the step (1) at one end of the PET biaxially oriented film 1, quickly and uniformly coating the casting solution on the surface of the PET biaxially oriented film 1 by using a scraper, pre-evaporating at 50 ℃ for 10 seconds, quickly transferring the coated PET biaxially oriented film 1 into a vacuum oven, heating and crosslinking at 60 ℃ for 5 hours, soaking in ethanol after crosslinking is completed, taking out, and drying by using nitrogen for later use.
(3)PVA@SiO2Preparation of hydrophilic coating 3
Preparing 15 wt% PVA aqueous solution, adding 0.05 wt% hydrophilic silica, uniformly dispersing, standing for defoaming, fixing the PET biaxial stretching film 1 on a heating table, and fixing the PVA @ SiO2The solution is uniformly coated on the surface of the PET biaxial stretching film 1 by a scraper at 100 ℃, and then the PET biaxial stretching film is placed in an oven at 80 ℃ for drying to obtain the PET composite film.
As can be seen from the static contact angle chart of the PET composite film in fig. 2, the initial contact angle of the PET composite film is small, and the PET composite film can absorb water on the surface within 3min, which indicates that the PET composite film has good hydrophilicity and water absorbability. An antifogging function test of the efficient water-absorbing antifogging PET composite film prepared by the hot water vapor method is shown in figure 3, under the condition of a constant-temperature water bath kettle at 60 ℃, water drops are fully distributed on the surface of the PET film which is not coated and modified after 90 minutes of water vapor action, the efficient water-absorbing antifogging PET composite film does not generate fogging phenomenon, good transparency is still kept, and long-acting and excellent antifogging performance is shown. From the test chart of FIG. 4, it can be seen that PVA @ SiO2The composite film of the/cellulose/PET biaxial stretching film 1 has high light transmittance and meets the standard of agricultural films.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art will understand that various changes, modifications and substitutions can be made without departing from the spirit and scope of the invention as defined by the appended claims. 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 (10)
1. A process for preparing the efficient water-absorbing antifogging agricultural PET composite film includes such steps as coating the corona-treated bidirectional PET film on itA cellulose high water absorption coating layer is coated with a PVA @ SiO layer2The hydrophilic coating forms a three-layer composite membrane structure, and is characterized by comprising the following steps:
step one, preparing a cellulose-based high-water-absorption casting solution, which comprises the following steps:
dissolving a certain amount of natural cellulose or carboxymethyl cellulose, adding monomers in proportion, stirring in a constant-temperature stirrer, heating the temperature to a specified temperature, adding a certain amount of initiator, carrying out the whole reaction under the protection of nitrogen, cooling the reaction temperature to room temperature after reacting for a period of time, adding a cross-linking agent N, N' -methylene bisacrylamide, stirring for 30 minutes at room temperature, adding a proper amount of distilled water to adjust to a proper viscosity, and stopping stirring, standing and defoaming for later use;
step two, preparing the cellulose high water absorption coating, which comprises the following steps:
fixing the cleaned PET biaxially oriented film on a heating table, extruding the casting solution prepared in the step one on one end of the PET biaxially oriented film, quickly and uniformly coating the casting solution on the surface of the PET biaxially oriented film by using a scraper, pre-evaporating for 10 seconds at a preset temperature, quickly transferring the coated PET biaxially oriented film into a vacuum oven for heating and crosslinking, soaking the film in ethanol after crosslinking is completed, taking out the film and drying the film by using nitrogen for later use;
step three, PVA @ SiO2The preparation of the hydrophilic coating is as follows:
dissolving PVA in distilled water, adding hydrophilic silicon dioxide, dispersing uniformly, standing for defoaming, fixing the PET biaxial stretching film coated with the cellulose super-absorbent coating prepared in the step two on a heating table, and fixing the PVA @ SiO2The solution is uniformly coated on the surface of the PET biaxial stretching film by a scraper at a certain temperature, and then the PET biaxial stretching film is placed in an oven at 80 ℃ for drying to obtain the high-efficiency water-absorbing antifogging agricultural PET composite film.
2. The preparation method of the agricultural PET composite film with high efficiency, water absorption and fog prevention as claimed in claim 1, wherein the cellulose used in the cellulose-based high water absorption film casting solution is natural cellulose and carboxymethyl cellulose, and the cellulose concentration is 0.2 wt% -8 wt%.
3. The preparation method of the agricultural PET composite film with high efficiency, water absorption and fog prevention as claimed in claim 1, wherein the cellulose-based high water absorption film casting solution is prepared by an aqueous solution polymerization method.
4. The preparation method of the agricultural PET composite film with high water absorption and fog resistance as claimed in claim 1, wherein the cellulose-based high water absorption casting solution adopts monomers selected from any one or more of (meth) acrylic acid, acrylamide, acrylonitrile, sodium p-styrenesulfonate and 2-acrylamide-2-methylpropanesulfonic acid in any proportion.
5. The preparation method of the agricultural PET composite film with high efficiency, water absorption and fog resistance as claimed in claim 1, wherein the reaction temperature of the cellulose-based high water absorption film casting solution is 55-80 ℃, and the reaction time is 1-10 hours.
6. The preparation method of the agricultural PET composite film with high water absorption and antifogging performance as claimed in claim 1, wherein the addition amount of the initiator of the cellulose-based high water absorption film casting solution is 0.5% -50% of the mass of the cellulose, and the addition amount of the cross-linking agent N, N' -methylene bisacrylamide is 0.5% -50%.
7. The preparation method of the agricultural PET composite film with high efficiency water absorption and fog prevention as claimed in claim 1, wherein the crosslinking temperature of the cellulose-based high water absorption coating is 50-150 ℃, and the crosslinking time is 0.5-24 hours.
8. The preparation method of the efficient water-absorbing antifogging agricultural PET composite film according to claim 1, wherein the pre-evaporation temperature of the cellulose-based high water-absorbing coating during coating is 30-150 ℃.
9. The preparation method of the efficient water-absorbing antifogging agricultural PET composite film according to claim 1, wherein PVA @ SiO is2The mass concentration of PVA in the hydrophilic coating is 3-20 wt%, and the mass concentration of water-based SiO2 is 0.01-15 wt%.
10. The preparation method of the efficient water-absorbing antifogging agricultural PET composite film according to claim 1, wherein PVA @ SiO is2The coating temperature of the hydrophilic coating is 25-150 ℃.
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