CN112592074B - Preparation method of aluminum phosphate super-hydrophilic film - Google Patents
Preparation method of aluminum phosphate super-hydrophilic film Download PDFInfo
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- CN112592074B CN112592074B CN202011466665.3A CN202011466665A CN112592074B CN 112592074 B CN112592074 B CN 112592074B CN 202011466665 A CN202011466665 A CN 202011466665A CN 112592074 B CN112592074 B CN 112592074B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
- C03C17/23—Oxides
- C03C17/25—Oxides by deposition from the liquid phase
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
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Abstract
The invention discloses a preparation method of an aluminum phosphate super-hydrophilic film, which comprises the following steps: s1, preparing aluminum phosphate sol, wherein the concentration of Al in the aluminum phosphate sol is 0.005-0.5 mol/L; s2, aging the aluminum phosphate sol; s3, plating an aluminum phosphate precursor film on the surface of the substrate by using the aged aluminum phosphate sol; s4, preheating the aluminum phosphate precursor film at 90-150 ℃ for 0.5-5 h; s5, heating the preheated aluminum phosphate precursor film at the temperature of 200-1000 ℃ for 0.5-5 h to obtain an aluminum phosphate super-hydrophilic film; the inorganic hydrophilic transparent film prepared by the method has good durability, super-hydrophilicity and good transmittance to visible light.
Description
Technical Field
The invention relates to the technical field of functional films, in particular to a preparation method of an aluminum phosphate super-hydrophilic film.
Background
Since the hydrophilic film has excellent properties such as stain resistance and antifogging property, it has been widely studied and applied in recent years. At present, the preparation of hydrophilic films is mainly divided into two directions, namely a high polymer material with hydrophilic groups and an inorganic photocatalytic material. The polymer material has poor durability in outdoor severe environment. The photocatalytic material needs to be excited to generate oxygen vacancy adsorption under certain ultraviolet or visible light, OH generates hydrophilic characteristic, and the photocatalytic material is typically TiO2A hydrophilic membrane. However, in the case of weak light or even no light, the hydrophilicity of the photocatalytic material becomes weak. Therefore, in view of durability and light dependence, the construction of inorganic non-photocatalytic hydrophilic membranes has important application value, but no report is found for the research on the aspect until now.
Disclosure of Invention
The invention aims to provide a preparation method of an aluminum phosphate super-hydrophilic film, and the inorganic hydrophilic transparent film prepared by the method has good durability, super-hydrophilicity and good transmittance to visible light.
The technical scheme adopted by the invention for solving the technical problem is as follows:
a preparation method of an aluminum phosphate super-hydrophilic film comprises the following steps:
s1, preparing aluminum phosphate sol, wherein the concentration of Al in the aluminum phosphate sol is 0.005-0.5 mol/L;
s2, aging the aluminum phosphate sol;
s3, plating an aluminum phosphate precursor film on the surface of the substrate by using the aged aluminum phosphate sol;
s4, preheating the aluminum phosphate precursor film at 90-150 ℃ for 0.5-5 h;
s5, heating the preheated aluminum phosphate precursor film at the temperature of 200-1000 ℃ for 0.5-5 h to obtain the aluminum phosphate super-hydrophilic film.
Further, when preparing the aluminum phosphate sol in step S1, dissolving an aluminum source and a phosphorus source in water, and then adding citric acid and polyethylene glycol to prepare the aluminum phosphate sol;
the aluminum source is one or more of aluminum lactate, aluminum acetate, aluminum chloride and aluminum nitrate; the phosphorus source is one or more of phosphoric acid, diammonium hydrogen phosphate and ammonium dihydrogen phosphate;
the citric acid meets the condition that the molar ratio of Al to the citric acid is 1: 1-1: 10;
the polyethylene glycol satisfies the condition that the molar ratio of Al to-OH is 1: 1-1: 10.
Further, the aging temperature in the aging step of S2 is 20-50 ℃, and the aging time is 0.5-72 h.
The invention also provides another preparation method of the aluminum phosphate super-hydrophilic film, which comprises the following steps:
s1, preparing aluminum phosphate sol, wherein the concentration of Al in the aluminum phosphate sol is 0.005-0.5 mol/L;
s2, aging the aluminum phosphate sol;
s3, drying the aged aluminum phosphate sol to obtain aluminum phosphate gel;
s4, preheating aluminum phosphate gel at 90-150 ℃ for 0.5-5 h;
s5, heating the preheated aluminum phosphate gel at 200-1000 ℃ for 0.5-5 h to obtain the aluminum phosphate super-hydrophilic film.
The aluminum phosphate has the beneficial effects that the aluminum phosphate has two special tetrahedrons of P-O and Al-O, the tetrahedrons are strictly and orderly arranged in an alternating mode to form a unique molecular structure, and a transparent film with a pore channel structure is easy to form; meanwhile, the formation of an aluminum phosphate pore channel structure is promoted under the action of an organic coordination agent in a sol-gel method, so that a hydrophilic film is easy to construct; the inorganic hydrophilic transparent film prepared by the method has good durability, super-hydrophilicity and good transmittance to visible light.
Drawings
The invention is further illustrated with reference to the following figures and examples:
FIG. 1 is a graph showing the hydrophilicity of an aluminum phosphate superhydrophilic thin film obtained in the first example of the present invention;
FIG. 2 is a graph showing the hydrophilicity of an aluminum phosphate superhydrophilic thin film obtained in example two of the present invention;
FIG. 3 is a graph showing the hydrophilicity of an aluminum phosphate superhydrophilic thin film obtained in example III of the present invention;
FIG. 4 is a graph showing the hydrophilicity of the aluminum phosphate superhydrophilic thin film obtained in example four of the present invention.
Detailed Description
Example one
The invention provides a preparation method of an aluminum phosphate super-hydrophilic film, which comprises the following steps:
s1, preparing aluminum phosphate sol, weighing 0.2205g of aluminum lactate, dissolving the aluminum lactate into 30ml of water, and respectively adding 1ml of 0.075mol/L phosphoric acid, 1.57g of citric acid and 0.465g of polyethylene glycol to obtain the aluminum phosphate sol;
s2, aging the aluminum phosphate sol for 24 hours at room temperature;
s3, plating an aluminum phosphate precursor film on the surface of the glass substrate by using the aged aluminum phosphate sol;
s4, preheating the aluminum phosphate precursor film at 100 ℃ for 30 min;
and S5, heating the preheated aluminum phosphate precursor film at 500 ℃ for 30min, and naturally cooling to room temperature to obtain the aluminum phosphate super-hydrophilic film.
And (3) carrying out a hydrophilicity test on the obtained aluminum phosphate super-hydrophilic film, wherein the contact angle is 1.4 degrees, as shown in figure 1.
Example two
The invention provides a preparation method of an aluminum phosphate super-hydrophilic film, which comprises the following steps:
s1, preparing aluminum phosphate sol, weighing 1.532g of aluminum isopropoxide, dissolving the aluminum isopropoxide into 30ml of water, and respectively adding 1ml of 0.075mol/L phosphoric acid, 1.57g of citric acid and 4.65g of polyethylene glycol to obtain the aluminum phosphate sol;
s2, aging the aluminum phosphate sol at room temperature for 6 hours;
s3, plating an aluminum phosphate precursor film on the surface of the glass substrate by using the aged aluminum phosphate sol;
s4, preheating the aluminum phosphate precursor film at 100 ℃ for 1 h;
and S5, heating the preheated aluminum phosphate precursor film at 500 ℃ for 1h, and naturally cooling to room temperature to obtain the aluminum phosphate super-hydrophilic film.
And (3) carrying out a hydrophilicity test on the obtained aluminum phosphate super-hydrophilic film, wherein the contact angle is 1.6 degrees, as shown in figure 2.
EXAMPLE III
The invention provides a preparation method of an aluminum phosphate super-hydrophilic film, which comprises the following steps:
s1, preparing aluminum phosphate sol, weighing 0.0441g of aluminum lactate, dissolving the aluminum lactate into 30ml of water, and respectively adding 0.2ml of 0.075mol/L phosphoric acid, 1.57g of citric acid and 0.465g of polyethylene glycol to obtain the aluminum phosphate sol;
s2, aging the aluminum phosphate sol for 0.5h at room temperature;
s3, drying the aged aluminum phosphate sol to obtain aluminum phosphate gel;
s4, preheating aluminum phosphate gel at 90 ℃ for 5 h;
and S5, heating the preheated aluminum phosphate precursor film at 500 ℃ for 1h, and naturally cooling to room temperature to obtain the aluminum phosphate super-hydrophilic film.
And (3) carrying out a hydrophilicity test on the obtained aluminum phosphate super-hydrophilic film, wherein the contact angle is 2.5 degrees, as shown in figure 3.
Example four
The invention provides a preparation method of an aluminum phosphate super-hydrophilic film, which comprises the following steps:
s1, preparing aluminum phosphate sol, weighing 4.41g of aluminum lactate, dissolving the aluminum lactate into 30ml of water, and respectively adding 20ml of 0.075mol/L phosphoric acid, 1.57g of citric acid and 4.65g of polyethylene glycol to obtain the aluminum phosphate sol;
s2, aging the aluminum phosphate sol for 24 hours at room temperature;
s3, plating an aluminum phosphate precursor film on the surface of the glass substrate by using the aged aluminum phosphate sol;
s4, preheating the aluminum phosphate precursor film at 100 ℃ for 30 min;
and S5, heating the preheated aluminum phosphate precursor film at 500 ℃ for 6h, and naturally cooling to room temperature to obtain the aluminum phosphate super-hydrophilic film.
And (3) carrying out a hydrophilicity test on the obtained aluminum phosphate super-hydrophilic film, wherein the contact angle is 3.1 degrees, as shown in figure 4.
The foregoing is merely a preferred embodiment of the invention and is not intended to limit the invention in any manner; those skilled in the art can make numerous possible variations and modifications to the present teachings, or modify equivalent embodiments to equivalent variations, without departing from the scope of the present teachings, using the methods and techniques disclosed above. Therefore, any simple modifications, equivalent substitutions, equivalent changes and modifications made to the above embodiments according to the technical essence of the present invention are within the scope of the technical scheme of the present invention.
Claims (4)
1. The preparation method of the aluminum phosphate super-hydrophilic film is characterized by comprising the following steps:
s1, preparing aluminum phosphate sol, wherein the concentration of Al in the aluminum phosphate sol is 0.005-0.5 mol/L;
s2, aging the aluminum phosphate sol;
s3, plating an aluminum phosphate precursor film on the surface of the substrate by using the aged aluminum phosphate sol;
s4, preheating the aluminum phosphate precursor film at 90-150 ℃ for 0.5-5 h;
s5, heating the preheated aluminum phosphate precursor film at the temperature of 200-1000 ℃ for 0.5-5 h to obtain the aluminum phosphate super-hydrophilic film.
2. The method for preparing the aluminum phosphate super-hydrophilic film as recited in claim 1, wherein the step S1 is to prepare the aluminum phosphate sol by dissolving the aluminum source and the phosphorus source in water, and then adding citric acid and polyethylene glycol to prepare the aluminum phosphate sol;
the aluminum source is one or more of aluminum lactate, aluminum acetate, aluminum chloride and aluminum nitrate; the phosphorus source is one or more of phosphoric acid, diammonium hydrogen phosphate and ammonium dihydrogen phosphate;
the citric acid meets the condition that the molar ratio of Al to the citric acid is 1: 1-1: 10;
the polyethylene glycol satisfies the condition that the molar ratio of Al to-OH is 1: 1-1: 10.
3. The method as recited in claim 1, wherein the aging temperature in the step S2 is 20-50 ℃ and the aging time is 0.5-72 h.
4. The preparation method of the aluminum phosphate super-hydrophilic film is characterized by comprising the following steps:
s1, preparing aluminum phosphate sol, wherein the concentration of Al in the aluminum phosphate sol is 0.005-0.5 mol/L;
s2, aging the aluminum phosphate sol;
s3, drying the aged aluminum phosphate sol to obtain aluminum phosphate gel;
s4, preheating aluminum phosphate gel at 90-150 ℃ for 0.5-5 h;
s5, heating the preheated aluminum phosphate gel at 200-1000 ℃ for 0.5-5 h to obtain the aluminum phosphate super-hydrophilic film.
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| CN113885265B (en) * | 2021-09-25 | 2024-06-18 | 中建材玻璃新材料研究院集团有限公司 | All-solid-state organic electrochromic composite film system intelligent glass component and preparation method thereof |
| CN114477117A (en) * | 2021-12-17 | 2022-05-13 | 中建材蚌埠玻璃工业设计研究院有限公司 | Aluminum phosphate-based powder for heat insulation and preparation method thereof |
| CN114477790B (en) * | 2021-12-24 | 2024-03-15 | 中建材玻璃新材料研究院集团有限公司 | Long-acting hydrophobic coating for glass and preparation method thereof |
| CN114326241B (en) * | 2021-12-27 | 2024-06-18 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of ion transmission layer and component composite film system for inorganic electrochromic |
| CN114213145B (en) * | 2021-12-27 | 2022-10-14 | 中建材玻璃新材料研究院集团有限公司 | Preparation method of foamed aluminum phosphate |
| CN115432937B (en) * | 2022-08-19 | 2024-03-12 | 中建材玻璃新材料研究院集团有限公司 | Aluminum phosphate film with micro-nano combined array and preparation method thereof |
| CN115818973A (en) * | 2022-12-02 | 2023-03-21 | 中建材玻璃新材料研究院集团有限公司 | Monolayer aluminum phosphate antireflection film in visible light band and preparation method thereof |
| CN115849727B (en) * | 2022-12-15 | 2024-01-12 | 中建材玻璃新材料研究院集团有限公司 | Aluminum phosphate film with reticular structure and preparation method thereof |
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| FR2117637A5 (en) * | 1970-12-11 | 1972-07-21 | Ici Ltd | Coating substrates - by applying compsn forming aluminium phosphate and drying under critical surface conditions and then curing to form aluminium phosphate |
| WO1993005199A1 (en) * | 1991-09-04 | 1993-03-18 | Furukawa Aluminum Co., Ltd. | Aluminum alloy sheet for automotive body and production thereof |
| CN1029220C (en) * | 1991-09-11 | 1995-07-05 | 中国石油化工总公司石油化工科学研究院 | Method for preparation of phosphorated aluminiferous collosol |
| US6461415B1 (en) * | 2000-08-23 | 2002-10-08 | Applied Thin Films, Inc. | High temperature amorphous composition based on aluminum phosphate |
| JP2002274823A (en) * | 2001-03-23 | 2002-09-25 | Asahi Kasei Corp | Method for producing aluminophosphate |
| CN100363454C (en) * | 2006-01-25 | 2008-01-23 | 浙江大学 | Production of antifogging and abrasive coating solution of spectacle lens |
| CN101792259A (en) * | 2010-03-17 | 2010-08-04 | 中国科学院上海光学精密机械研究所 | Mesoporous aluminum phosphate glass with high specific surface area and preparation method thereof |
| CN107500261B (en) * | 2017-08-23 | 2019-12-24 | 广西新晶科技有限公司 | Aluminum metaphosphate powder for optical glass and preparation method thereof |
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