CN112940324B - Preparation method of efficient water-absorbing anti-fog agricultural PET composite film - Google Patents
Preparation method of efficient water-absorbing anti-fog agricultural PET composite film Download PDFInfo
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Abstract
The invention discloses a preparation method of an efficient water-absorbing anti-fog agricultural PET composite film, which is of a three-layer structure, wherein a PET biaxially oriented film after corona is used as a matrix, a modified cellulose high water-absorbing coating layer is coated on the surface of the matrix to be a water-absorbing layer, and then a PVA@SiO layer is coated on the surface of the matrix 2 The 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, and comprises (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@SiO 2 The 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 anti-fog, 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 efficient water-absorbing antifogging agricultural PET composite film.
Background
The traditional PE and PVC agricultural film has high light transmittance and low price, but the large temperature difference change in severe cold areas and winter causes the weather resistance and mechanical properties of the existing agricultural film to be poor, the anti-fog function is lost, the light transmittance is reduced, the growth of crops is affected, and the use time is greatly shortened, so that the use of the agricultural film is severely limited. Meanwhile, as petroleum resources are gradually exhausted, the problem of environmental pollution attracts attention, and white pollution caused by agricultural film products such as polyethylene, polyvinyl chloride and the like to cultivated lands is also urgently needed to be solved by researching and developing novel green recyclable agricultural film products.
The biaxially oriented PET film has high strength, good transparency and good weather resistance, can be used for a long time at low temperature, is environment-friendly, pollution-free and recyclable, is preferable as a novel agricultural film, is easy to fog, and is a primary problem to be solved as an agricultural film anti-fog drop.
Disclosure of Invention
The invention aims to provide a preparation method of an efficient water-absorbing anti-fog agricultural PET composite film, which aims to solve the problems in the background technology.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a preparation method of an efficient water-absorbing anti-fog agricultural PET composite film comprises the steps that a substrate is a PET biaxially oriented film subjected to corona treatment, a cellulose high-water-absorbing coating layer is coated on the PET biaxially oriented film, and then a PVA@SiO layer is coated on the PET biaxially oriented film 2 The hydrophilic coating forms a three-layer composite membrane structure, and is characterized by comprising the following steps:
step one, preparing a cellulose-based super absorbent casting solution, which comprises the following steps:
dissolving a certain amount of natural cellulose or carboxymethyl cellulose, adding monomers according to a 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 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, regulating to a proper viscosity, stopping stirring, standing and defoaming for standby;
step two, preparing a cellulose super absorbent coating, which comprises the following steps:
fixing the cleaned PET biaxially oriented film on a heating table, extruding the casting film liquid prepared in the first step on one end of the PET biaxially oriented film, coating the casting film liquid on the surface of the PET biaxially oriented film uniformly by using a scraper, pre-evaporating for 10 seconds at a preset temperature, transferring the coated PET biaxially oriented film into a vacuum oven for heating and crosslinking, soaking in ethanol after crosslinking is finished, taking out, and drying with nitrogen for standby;
step three, PVA@SiO 2 The preparation of the hydrophilic coating is specifically as follows:
dissolving PVA in distilled water, adding hydrophilic silicon dioxide, dispersing uniformly, standing for defoaming, fixing the PET biaxially oriented film coated with the cellulose high water absorption coating prepared in the second step on a heating table, and obtaining PVA@SiO 2 The solution is uniformly coated on the surface of the PET biaxially oriented film by a scraper at a certain temperature, and then the PET biaxially oriented film is placed in an oven at 80 ℃ for drying to obtain the efficient water-absorbing anti-fog agricultural PET composite film.
Furthermore, the cellulose used in the cellulose-based super absorbent casting solution is natural cellulose and carboxymethyl cellulose, and the concentration of the cellulose is 0.2-8wt%.
Furthermore, the cellulose-based super absorbent casting solution adopts an aqueous solution polymerization method.
Further, the cellulose-based super absorbent casting solution adopts any one or more of (methyl) acrylic acid, acrylamide, acrylonitrile, sodium p-styrenesulfonate and 2-acrylamide-2-methylpropanesulfonic acid according to any proportion.
Further, the reaction temperature of the cellulose-based super absorbent casting solution is 55-80 ℃ and the reaction time is 1-10 hours.
Further, the addition amount of the initiator of the cellulose-based super absorbent casting film liquid is 0.5-50% of the mass of 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 ℃ when the cellulose-based super absorbent coating is coated.
Further, the PVA@SiO 2 The mass concentration of PVA in the hydrophilic coating is 3-20wt%, and the hydrophilic coating is aqueous SiO 2 The mass concentration of (2) is 0.01wt% to 15wt%.
Further, PVA@SiO in the third step 2 The 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@SiO 2 The 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 anti-fog, adopts an industrialized film surface coating process, has the advantages of simple operation, wide raw material sources, low price, environmental protection, no pollution, recoverability, high light transmittance of the composite film, obvious anti-fog effect, difficult failure and long-time use at low temperature, 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 that are 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 other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a schematic diagram of the PET composite film structure of the present invention;
fig. 2 is a graph of contact angle of the high-efficiency water-absorbing anti-fog agricultural PET composite film prepared in example 1.
Fig. 3 is an anti-fog property test chart of the high-efficiency water-absorbing anti-fog agricultural PET composite film prepared in example 1.
Fig. 4 is a graph of light transmittance of each product of example 1.
Reference numerals:
1. PET biaxially oriented film; 2. a cellulose superabsorbent coating; 3. PVA@SiO 2 A hydrophilic coating.
Detailed Description
The invention is further described in connection with the following detailed description:
example 1
(1) Preparation of cellulose-based super-absorbent casting film liquid
Dissolving 0.2g of cellulose in 7% NaOH/12% urea aqueous solution, adding 1g of acrylamide, starting stirring, heating 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, adding 0.007g 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 standby.
(2) Preparation of cellulose superabsorbent coating 2
Fixing the cleaned PET biaxially oriented film 1 on a heating table, extruding the casting film liquid prepared in the step (1) at one end of the PET biaxially oriented film 1, coating the casting film liquid on the surface of the PET biaxially oriented film 1 uniformly by using a scraper, pre-evaporating for 10 seconds at 50 ℃, transferring the coated PET biaxially oriented film 1 into a vacuum oven, heating and crosslinking for 4 hours at 60 ℃, soaking in ethanol after crosslinking, taking out, and drying with nitrogen for later use.
(3)PVA@SiO 2 Preparation of hydrophilic coating 3
Preparing 11wt% PVA aqueous solution, adding 0.05wt% hydrophilic silica, dispersing uniformly, standing for defoaming, fixing PET biaxially oriented film on a heating table, and obtaining PVA@SiO 2 The solution is uniformly coated on the surface of the PET biaxially oriented film 1 by a scraper at the temperature of 100 ℃, and then the PET biaxially oriented film is placed in an oven at the temperature of 80 ℃ for drying.
Example 2
(1) Preparation of cellulose-based super-absorbent casting film liquid
Dissolving 0.2g of carboxymethyl cellulose in 9.8g of distilled water, adding 2g of acrylic acid with the neutralization degree of 75%, 0.040g 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, 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 standby.
(2) Preparation of cellulose superabsorbent coating 2
Fixing the cleaned PET biaxially oriented film 1 on a heating table, extruding the casting film liquid prepared in the step (1) at one end of the PET biaxially oriented film 1, coating the casting film liquid on the surface of the PET biaxially oriented film 1 uniformly by using a scraper, pre-evaporating for 10 seconds at 50 ℃, transferring the coated PET biaxially oriented film 1 into a vacuum oven, heating and crosslinking for 4 hours at 60 ℃, soaking in ethanol after crosslinking, taking out, and drying with nitrogen for later use.
(3)PVA@SiO 2 Preparation of hydrophilic coating 3
Preparing 11wt% PVA aqueous solution, adding 0.05wt% hydrophilic silica, dispersing uniformly, standing for defoaming, fixing the PET biaxially oriented film 1 on a heating table, and obtaining PVA@SiO 2 The solution is uniformly coated on the surface of the PET biaxially oriented film 1 by a scraper at the temperature of 100 ℃, and then the PET biaxially oriented film is placed in an oven at the temperature of 80 ℃ for drying to obtain the PET composite film.
Example 3
(1) Preparation of cellulose-based super-absorbent casting film liquid
Dissolving 0.2g of cellulose in 7% NaOH/12% urea aqueous solution, adding 0.5g of acrylamide, starting stirring, heating 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, adding 0.005g of cross-linking agent N, N' -methylenebisacrylamide, stirring for 30 minutes at room temperature, adding distilled water to adjust to a proper viscosity, stopping stirring, standing and defoaming for standby.
(2) Preparation of cellulose superabsorbent coating 2
Fixing the cleaned PET biaxially oriented film 1 on a heating table, extruding the casting film liquid prepared in the step (1) at one end of the PET biaxially oriented film 1, coating the casting film liquid on the surface of the PET biaxially oriented film 1 uniformly by using a scraper, pre-evaporating for 10 seconds at 50 ℃, transferring the coated PET biaxially oriented film 1 into a vacuum oven, heating and crosslinking for 4 hours at 70 ℃, soaking in ethanol after crosslinking, taking out, and drying with nitrogen for later use.
(3)PVA@SiO 2 Preparation of hydrophilic coating 3
Preparing 5wt% PVA aqueous solution, adding 0.05wt% hydrophilic silica, dispersing uniformly, standing for defoaming, fixing PET biaxially oriented film on a heating table, and obtaining PVA@SiO 2 The solution is uniformly coated on the surface of the PET biaxially oriented film 1 by a scraper at the temperature of 100 ℃, and then the PET biaxially oriented film is placed in an oven at the temperature of 80 ℃ for drying.
Example 4
(1) Preparation of cellulose-based super-absorbent casting film liquid
Dissolving 0.2g of carboxymethyl cellulose in 9.8g of distilled water, adding 2g of acrylic acid with the neutralization degree of 75%, 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, adding 0.008g of cross-linking agent N, N' -methylene bisacrylamide, stirring for 60 minutes at room temperature, adding distilled water to adjust to proper viscosity, stopping stirring, standing and defoaming for standby.
(2) Preparation of cellulose superabsorbent coating 2
Fixing the cleaned PET biaxially oriented film 1 on a heating table, extruding the casting film liquid prepared in the step (1) at one end of the PET biaxially oriented film 1, coating the casting film liquid on the surface of the PET biaxially oriented film 1 uniformly by using a scraper, pre-evaporating for 10 seconds at 50 ℃, transferring the coated PET biaxially oriented film 1 into a vacuum oven, heating and crosslinking for 5 hours at 60 ℃, soaking in ethanol after crosslinking, taking out, and drying with nitrogen for later use.
(3)PVA@SiO 2 Preparation of hydrophilic coating 3
Preparing 15wt% PVA aqueous solution, adding 0.05wt% hydrophilic silicon dioxide, dispersing uniformly, standing for defoaming, fixing the PET biaxially oriented film 1 on a heating table, and obtaining PVA@SiO 2 The solution is uniformly coated on the surface of the PET biaxially oriented film 1 by a scraper at the temperature of 100 ℃, and then the PET biaxially oriented film is placed in an oven at the temperature of 80 ℃ for drying to obtain the PET composite film.
From the static contact angle diagram of the PET composite film in FIG. 2, it can be seen that the initial contact angle of the PET composite film is smaller, and the PET composite film can be used for surface treatment within 3minIndicating that it has good hydrophilicity and water absorbability. The anti-fog function test of the efficient water-absorbing anti-fog PET composite film prepared by adopting the hot water steam method is shown in figure 3, under the condition of a 60 ℃ constant-temperature water bath kettle, water drops are fully distributed on the surface of the PET film which is not coated and modified after the effect of the water steam for 90 minutes, the efficient water-absorbing anti-fog PET composite film does not generate the phenomenon of fog, and still keeps good transparency, and long-acting and excellent anti-fog performance is shown. From the graph of the transmittance of FIG. 4, PVA@SiO can be seen 2 The cellulose/PET biaxially oriented film 1 composite film has high light transmittance and meets the standards of agricultural films.
Finally, it should be noted that: the foregoing description is only a preferred embodiment of the present invention, and the present invention is not limited to the above-described embodiment, but may be modified or substituted for some of the technical features described in the above-described embodiments by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (9)
1. A preparation method of an efficient water-absorbing anti-fog agricultural PET composite film comprises the steps that a substrate is a PET biaxially oriented film subjected to corona treatment, a cellulose high-water-absorbing coating layer is coated on the PET biaxially oriented film, and then a PVA@SiO layer is coated on the PET biaxially oriented film 2 The hydrophilic coating forms a three-layer composite membrane structure, and is characterized by comprising the following steps:
step one, preparing a cellulose-based super absorbent casting solution, which comprises the following steps:
dissolving a certain amount of natural cellulose or carboxymethyl cellulose, adding monomers according to a proportion, stirring in a constant-temperature stirrer, heating the temperature to a reaction 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 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, regulating to a proper viscosity, stopping stirring, standing and defoaming for standby; the monomer is any one or more of (methyl) acrylic acid, acrylamide, acrylonitrile, sodium p-styrenesulfonate and 2-acrylamide-2-methylpropanesulfonic acid in any proportion;
step two, preparing a cellulose super absorbent coating, which comprises the following steps:
fixing the cleaned PET biaxially oriented film on a heating table, extruding the casting film liquid prepared in the first step on one end of the PET biaxially oriented film, coating the casting film liquid on the surface of the PET biaxially oriented film uniformly by using a scraper, pre-evaporating for 10 seconds at a preset temperature, transferring the coated PET biaxially oriented film into a vacuum oven for heating and crosslinking, soaking in ethanol after crosslinking is finished, taking out, and drying with nitrogen for standby;
step three, PVA@SiO 2 The preparation of the hydrophilic coating is specifically as follows:
dissolving PVA in distilled water, adding hydrophilic silicon dioxide, dispersing uniformly, standing for defoaming, fixing the PET biaxially oriented film coated with the cellulose high water absorption coating prepared in the second step on a heating table, and obtaining PVA@SiO 2 The solution is uniformly coated on the surface of the PET biaxially oriented film by a scraper at a certain temperature, and then the PET biaxially oriented film is placed in an oven at 80 ℃ for drying to obtain the efficient water-absorbing anti-fog agricultural PET composite film.
2. The preparation method of the efficient water-absorbing anti-fog agricultural PET composite film, according to claim 1, wherein the cellulose used in the cellulose-based super-absorbent casting film liquid is natural cellulose and carboxymethyl cellulose, and the cellulose concentration is 0.2-8wt%.
3. The method for preparing the efficient water-absorbing anti-fog agricultural PET composite film, which is disclosed in claim 1, wherein the cellulose-based super-absorbent casting film liquid adopts an aqueous solution polymerization method.
4. The method for preparing the efficient water-absorbing anti-fog agricultural PET composite film according to claim 1, wherein the reaction temperature of the cellulose-based super-absorbent casting film solution is 55-80 ℃ and the reaction time is 1-10 hours.
5. The preparation method of the efficient water-absorbing anti-fog agricultural PET composite film, which is disclosed in claim 1, wherein the addition amount of the initiator of the cellulose-based super-absorbent casting film liquid is 0.5-50% of the mass of cellulose, and the addition amount of the cross-linking agent N, N' -methylene bisacrylamide is 0.5-50% of the mass of cellulose.
6. The method for preparing the efficient water-absorbing anti-fog agricultural PET composite film according to claim 1, wherein the crosslinking temperature of the cellulose-based super absorbent coating is 50-150 ℃ and the crosslinking time is 0.5-24 hours.
7. The method for preparing the efficient water-absorbing and anti-fog agricultural PET composite film, which is disclosed in claim 1, wherein the pre-evaporation temperature of the cellulose-based super absorbent coating is 30-150 ℃ when the cellulose-based super absorbent coating is coated.
8. The method for preparing the efficient water-absorbing anti-fog agricultural PET composite film according to claim 1, wherein PVA@SiO 2 The mass concentration of PVA in the hydrophilic coating is 3-20wt%, and the hydrophilic coating is aqueous SiO 2 The mass concentration of (2) is 0.01wt% to 15wt%.
9. The method for preparing the efficient water-absorbing anti-fog agricultural PET composite film according to claim 1, wherein PVA@SiO 2 The coating temperature of the hydrophilic coating is 25-150 ℃.
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