Preparation method of laminated film with hydrophilicity

Abstract

The invention discloses a preparation method of a hydrophilic laminated film, and belongs to the technical field of film coating. The film prepared by using a liquid phase method is divided into a titanium dioxide layer film and an aluminum phosphate layer film, compared with a single-layer film, the uniformity is better, the titanium dioxide layer film has higher photocatalytic activity during ultraviolet irradiation, can degrade organic pollutants and is very strong in hydrophilicity, and a hydrophilic angle is quickly enlarged and spread to play transparent and self-cleaning roles; aluminum phosphate has two special tetrahedral structures of P-O and Al-O which are strictly, orderly and alternately arranged to form a unique molecular structure, a hydrophilic film with a pore channel structure is easily formed, the hydrophilic film and a titanium dioxide layer film can have a synergistic effect, the hydrophilicity of the laminated film is enhanced, a pulling method is used for coating, the operation is simple, and the uniformity of the film can be effectively improved; therefore, the prepared film is excellent in hydrophilic performance and good in self-cleaning effect and uniformity, and has important application value in the technical field of film coating.

Description

Technical Field

[0001] The invention belongs to the technical field of film coating, and in particular relates to a method for preparing a hydrophilic laminated film. Background Art

[0002] With the advancement of science and technology and the improvement of people's quality of life, hydrophilic film, as a functional material, has gradually gained favor in the market. It can not only improve the surface properties of materials, increase the comfort and service life of products, but also play a unique protective role in specific environments. For example, on the solar photovoltaic cover glass, the hydrophilic film has a self-cleaning function, which significantly reduces the cleaning and maintenance costs of photovoltaic modules.

[0003] At present, the hydrophilic film is commonly used as a water-based aluminum phosphate film. However, for the water-based aluminum phosphate film coating solution, direct coating on glass may reduce the uniformity of the film, resulting in incomplete coverage of the film on the glass, resulting in reduced film performance. Therefore, it is urgent to solve this problem to meet the higher demands in the field of coating technology. Summary of the invention

[0004] The purpose of the present invention is to overcome the defects of the prior art and provide a method for preparing aluminum titanate nanofibers.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] A method for preparing a hydrophilic laminated film comprises the following steps:

[0007] S1. Cut glass as a coating substrate, wipe it with a dust-free cloth, then immerse the cut glass in acetone, sodium ethoxide ethanol solution and hydrochloric acid aqueous solution in turn, and finally put it into water, use ultrasonic cleaning to remove residual cleaning liquid and impurities on the glass, and obtain a glass substrate;

[0008] S2, ethanol and acetylacetone were mixed, stirred and heated for 30 minutes, tetrabutyl titanate was added, and after stirring for another 30 minutes, an appropriate amount of deionized water was added, and the pH of the system was adjusted with a hydrochloric acid solution, and then N,N-dimethylformamide was added, and stirring was continued for 3 hours, and aged for 48 hours to obtain a titanium dioxide sol;

[0009] S3, mixing phosphoric acid and water and stirring for 30 minutes, adding aluminum dihydrogen phosphate, stirring evenly, adding polyethylene glycol, and finally adding sodium dodecyl sulfate and citric acid, continuing to stir for 2 hours, and letting it stand for 24 hours to obtain an aluminum phosphate coating solution;

[0010] The aluminum phosphate coating solution prepared by using aluminum-containing chemicals as raw materials, adding long-chain humidifiers such as polyethylene glycol and sodium dodecyl sulfate ionic surfactants with water as solvent has better uniformity and more balanced film thickness.

[0011] S4. Immerse the glass substrate obtained in step S1 into the titanium dioxide sol obtained in step S2, then lift the substrate material and dry it at 120°C, and then heat treat it at 450°C after drying. After the bottom film is cooled, immerse the substrate material in the aluminum phosphate coating solution again, and then slowly lift the substrate material again and let it stand at 30°C for 30 minutes. After solidification, heat treat it at 350°C and cool it to obtain a hydrophilic laminated film.

[0012] Furthermore, in step S2, the molar ratio of ethanol to tetrabutyl titanate is 60:1.

[0013] Furthermore, in step S2, the molar ratio of tetrabutyl titanate to acetylacetone is 1:1.

[0014] Furthermore, in step S2, the molar ratio of deionized water to tetrabutyl titanate is 4:1.

[0015] Furthermore, in step S2, the mass fraction of the hydrochloric acid solution is 6-12%, and the pH of the system is adjusted to 1-2.

[0016] Furthermore, in step S3, the ratio of phosphoric acid, water, aluminum dihydrogen phosphate, polyethylene glycol, sodium dodecyl sulfate and citric acid is 10 g:100 mL:12 g:5 g:2 g:2 g.

[0017] Furthermore, the molecular weight of the polyethylene glycol in step S3 is 800-1000.

[0018] Furthermore, in step S4, the pulling speed is 1000-2000 μm / s.

[0019] The prepared hydrophilic laminated film is divided into a titanium dioxide layer film and an aluminum phosphate layer film. The titanium dioxide layer film has a high photocatalytic activity when irradiated with ultraviolet light, can degrade organic pollutants, and has a strong hydrophilicity. The hydrophilic angle quickly increases and spreads out to play a transparent and self-cleaning role. Aluminum phosphate has two special PO and Al-O tetrahedral structures that are strictly ordered and alternately arranged to form a unique molecular structure, which is easy to form a hydrophilic film with a pore structure, and can synergize with the titanium dioxide layer film to enhance the hydrophilicity of the laminated film. In addition, this double-layer film structure has better uniformity than a single-layer film.

[0020] Beneficial effects of the present invention:

[0021] 1. The film prepared by the present invention is divided into a titanium dioxide film and an aluminum phosphate film, wherein the hydrophilicity is very strong and the self-cleaning effect is good; the aluminum phosphate film can synergize with the titanium dioxide film to enhance the hydrophilicity of the laminated film and has good uniformity;

[0022] 2. By adjusting the pH value with acid to control the hydrolysis rate and using the Czochralski method for coating, it is not only simple to operate, but also can effectively improve the uniformity of the film;

[0023] Therefore, the film prepared by the present invention has excellent hydrophilicity, good self-cleaning effect and uniformity, and has important application value in the field of film coating technology. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] The present invention will be further described below in conjunction with the accompanying drawings.

[0025] Figure 1 This is a diagram of the film structure of the present invention.

[0026] Figure 2 It is a coating process flow chart of the present invention.

[0027] Figure 3 This is a static water contact angle test diagram of Example 1 of the present invention. DETAILED DESCRIPTION

[0028] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0029] Example 1

[0030] according to Figure 2 The steps shown in the flow chart are to prepare a hydrophilic laminate film:

[0031] S1. Cut a 40×75 mm glass as a coating substrate, wipe it with a dust-free cloth, and then immerse the glass substrate in acetone, sodium ethoxide ethanol solution, and hydrochloric acid aqueous solution in sequence, and finally put it into water, and use ultrasonic cleaning to remove the residual cleaning solution and impurities on the glass to obtain a glass substrate;

[0032] S2, 276g of ethanol and 28g of acetylacetone were mixed, stirred and heated for 30min, 34g of tetrabutyl titanate was added, and 40g of deionized water was added after stirring for 30min, and the pH of the system was adjusted to 1 with hydrochloric acid solution (mass fraction of 6%), and then N,N-dimethylformamide was added, and stirring was continued for 3h, and aged for 48h to obtain titanium dioxide sol;

[0033] S3, 10g phosphoric acid and 100mL water were mixed and stirred for 30min, 12g aluminum dihydrogen phosphate was added, 5g polyethylene glycol (molecular weight 800) was added after stirring evenly, and finally 2g sodium dodecyl sulfate and 2g citric acid were added, stirring was continued for 2h, and the mixture was left to stand for 24h to obtain aluminum phosphate coating solution;

[0034] S4. Immerse the glass substrate obtained in step S1 into the titanium dioxide sol obtained in step S2, then pull up (pulling speed is 1000 μm / s) the substrate material and dry it at 120°C, and then heat treat it at 450°C after drying. After the bottom film is cooled, immerse the substrate material in the aluminum phosphate plating solution again, and then slowly lift up the substrate material again and let it stand at 30°C for 30 minutes. After solidification, heat treat it at 350°C and cool it to obtain a hydrophilic laminated film.

[0035] Example 2

[0036] according to Figure 2 The steps shown in the flow chart are to prepare a hydrophilic laminate film:

[0037] S1. Cut a 40×75 mm glass as a coating substrate, wipe it with a dust-free cloth, and then immerse the glass substrate in acetone, sodium ethoxide ethanol solution, and hydrochloric acid aqueous solution in sequence, and finally put it into water, and use ultrasonic cleaning to remove the residual cleaning solution and impurities on the glass to obtain a glass substrate;

[0038] S2, 552g of ethanol and 28g of acetylacetone were mixed, stirred and heated for 30min, 68g of tetrabutyl titanate was added, and then 80g of deionized water was added after stirring for 30min, and the pH of the system was adjusted to 2 with hydrochloric acid solution (mass fraction of 12%), and then N,N-dimethylformamide was added, and stirring was continued for 3h, and aged for 48h to obtain titanium dioxide sol;

[0039] S3, 2g phosphoric acid and 200mL water were mixed and stirred for 30min, 24g aluminum dihydrogen phosphate was added, 10g polyethylene glycol (molecular weight 1000) was added after stirring evenly, and finally 4g sodium dodecyl sulfate and 4g citric acid were added, stirring was continued for 2h, and the aluminum phosphate coating solution was obtained after standing for 24h;

[0040] S4. Immerse the glass substrate obtained in step S1 into the titanium dioxide sol obtained in step S2, then pull up (pulling speed is 2000 μm / s) the substrate material and dry it at 120°C, and then heat treat it at 450°C after drying. After the bottom film is cooled, immerse the substrate material in the aluminum phosphate plating solution again, and then slowly lift up the substrate material again and let it stand at 30°C for 30 minutes. After solidification, heat treat it at 350°C and cool it to obtain a hydrophilic laminated film.

[0041] The contact angle of the hydrophilic laminated film obtained in Example 1 was measured. The test results are as follows: Figure 3As shown, the contact angle is 85.75°, which is less than 90°. Therefore, the film prepared by the present invention has excellent hydrophilicity, good self-cleaning effect and uniformity, and has important application value in the field of film coating technology.

[0042] In the description of the specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0043] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.

Claims

1. A method for preparing a hydrophilic laminated film, characterized in that: The following steps are involved: S1, cutting glass as a coating substrate, and then immersing the cut glass in acetone, sodium ethoxide ethanol solution and hydrochloric acid aqueous solution in sequence, and finally putting it into water for washing to obtain a glass substrate; S2, ethanol and acetylacetone were mixed, stirred and heated for 30 minutes, tetrabutyl titanate was added, and after stirring for another 30 minutes, an appropriate amount of deionized water was added, and the pH of the system was adjusted with a hydrochloric acid solution, and then N,N-dimethylformamide was added, and stirring was continued for 3 hours, and aged for 48 hours to obtain a titanium dioxide sol; S3, mixing phosphoric acid and water and stirring for 30 minutes, adding aluminum dihydrogen phosphate, stirring evenly, adding polyethylene glycol, and finally adding sodium dodecyl sulfate and citric acid, continuing to stir for 2 hours, and letting it stand for 24 hours to obtain an aluminum phosphate coating solution; S4. Immerse the glass substrate obtained in step S1 into the titanium dioxide sol obtained in step S2, then lift the substrate material and dry it at 120°C, and then heat treat it at 450°C after drying. After the bottom film is cooled, immerse the substrate material in the aluminum phosphate coating solution again, and then slowly lift the substrate material again and let it stand at 30°C for 30 minutes. After solidification, heat treat it at 350°C and cool it to obtain a hydrophilic laminated film.

2. The method for preparing a hydrophilic laminated film according to claim 1, characterized in that: In step S2, the molar ratio of ethanol to tetrabutyl titanate is 60:

1.

3. The method for preparing a hydrophilic laminated film according to claim 1, characterized in that: In step S2, the molar ratio of tetrabutyl titanate to acetylacetone is 1:

1.

4. The method for preparing a hydrophilic laminated film according to claim 1, characterized in that: In step S2, the molar ratio of deionized water to tetrabutyl titanate is 4:

1.

5. The method for preparing a hydrophilic laminated film according to claim 1, characterized in that: In step S2, the mass fraction of the hydrochloric acid solution is 6-12%, and the pH of the system is adjusted to 1-2.

6. The method for preparing a hydrophilic laminated film according to claim 1, characterized in that: In step S3, the ratio of phosphoric acid, water, aluminum dihydrogen phosphate, polyethylene glycol, sodium dodecyl sulfate and citric acid is 10g:100mL:12g:5g:2g:2g.

7. The method for preparing a hydrophilic laminated film according to claim 1, characterized in that: The molecular weight of the polyethylene glycol in step S3 is 800-1000.

8. The method for preparing a hydrophilic laminated film according to claim 1, characterized in that: The pulling speed in step S4 is 1000-2000 μm / s.

Images