CN111187528A - Hydrophobic anti-aging glass film and preparation method thereof - Google Patents
Hydrophobic anti-aging glass film and preparation method thereof Download PDFInfo
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- CN111187528A CN111187528A CN202010224555.XA CN202010224555A CN111187528A CN 111187528 A CN111187528 A CN 111187528A CN 202010224555 A CN202010224555 A CN 202010224555A CN 111187528 A CN111187528 A CN 111187528A
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Abstract
The invention relates to a hydrophobic anti-aging glass film and a preparation method thereof, belonging to the technical field of preparation of special film layers. The preparation method comprises the steps of firstly taking titanium isopropoxide as a raw material, reacting the titanium isopropoxide with acid for hydrolysis to prepare nano titanium sol, then modifying the nano titanium sol by using trimethylchlorosilane to obtain modified titanium sol, carrying out extraction heat treatment on the modified titanium sol to form a pretreated glass membrane, reacting sodium silicate with phosphoric acid to generate an orthosilicic acid reaction liquid, adding nano montmorillonite into the orthosilicic acid reaction liquid, heating and hydrolyzing to prepare needle-punched composite microspheres, blending the needle-punched composite microspheres, thermosetting acrylic resin and other raw materials to prepare the self-made waterproof aging-resistant coating, coating the coating on the surface of the pretreated glass membrane, and then carrying out thermal curing to finally prepare the hydrophobic aging-resistant glass membrane, wherein the hydrophobic aging-resistant glass membrane has wide application prospect.
Description
Technical Field
The invention relates to a hydrophobic anti-aging glass film and a preparation method thereof, belonging to the technical field of preparation of special film layers.
Background
At present, many glass products on the market need to be exposed to a severe environment for a long time and are easy to age and damage, but in order to meet the use requirements of some special occasions, the glass also needs to have certain hydrophobicity, and most of the existing glasses do not have the functions.
In view of the above-mentioned drawbacks, the present inventors have made active research and innovation to create a hydrophobic aging-resistant glass film and a method for preparing the same, which can impart both aging-resistant and hydrophobic effects to the glass surface after use.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a hydrophobic anti-aging glass film and a preparation method thereof.
The hydrophobic anti-aging glass film is prepared by coating a self-made waterproof anti-aging coating on the surface of a pretreated glass film and then thermally curing the coating,
the pretreated glass film is prepared by dipping, lifting and heat treatment of modified titanium sol;
the modified titanium sol is prepared by reacting titanium isopropoxide, butanol, a nitric acid solution, deionized water and trimethylchlorosilane;
the self-made waterproof anti-aging coating is prepared by reacting thermosetting acrylic resin, needle-punched composite microspheres, isopropanol, propylene glycol monolaurate and an ethanol solution;
the needle-punched composite microspheres are prepared by reacting reaction liquid with nano montmorillonite;
the reaction solution is prepared by reacting a sodium silicate solution with a phosphoric acid solution.
A preparation method of a hydrophobic anti-aging glass film comprises the following specific preparation steps:
(1) preparing modified titanium sol: mixing titanium isopropoxide and butanol, performing ultrasonic dispersion, adding a nitric acid solution and deionized water, hydrolyzing to obtain a titanium sol, and mixing the titanium sol and trimethylchlorosilane to obtain a modified titanium sol;
(2) preparation of a pretreated glass film: immersing glass to be treated into the modified titanium sol, standing, lifting, performing heat treatment after each film is immersed and pulled for 5 times to obtain a pretreated glass film;
(3) preparation of reaction solution: mixing a sodium silicate solution and a phosphoric acid solution, and carrying out ultrasonic oscillation reaction to obtain a reaction solution;
(4) preparing the needle-punched composite microspheres: mixing the reaction liquid with the nano montmorillonite, heating and stirring for reaction to obtain the needle-punched composite microspheres;
(5) preparing a self-made waterproof anti-aging coating: weighing thermosetting acrylic resin, needle-punched composite microspheres, isopropanol, propylene glycol monolaurate and ethanol solution, grinding, mixing and discharging to obtain the self-made waterproof anti-aging coating;
(6) preparing a hydrophobic anti-aging glass film: and (3) coating the self-made waterproof anti-aging coating on the surface of the pretreated glass film, and performing thermocuring to obtain the hydrophobic anti-aging glass film.
Further, the preparation method comprises the following specific steps:
(1) preparing modified titanium sol: mixing titanium isopropoxide and butanol, placing the mixture into an ultrasonic disperser for ultrasonic dispersion to obtain a precursor solution, adding a nitric acid solution and deionized water into the precursor solution, transferring the precursor solution into a water bath, stirring and hydrolyzing to obtain titanium sol, and mixing the obtained titanium sol and trimethylchlorosilane to obtain modified titanium sol;
(2) preparation of a pretreated glass film: immersing glass to be treated in the modified titanium sol, standing, vertically lifting the glass upwards, immediately placing the glass in a muffle furnace after each immersion lifting of one layer of film, performing heat treatment, and repeating for 5 times to obtain a pretreated glass film;
(3) preparation of reaction solution: mixing a sodium silicate solution and a phosphoric acid solution to obtain a mixed solution, loading the mixed solution into an ultrasonic oscillator, and carrying out ultrasonic oscillation reaction to obtain a reaction solution;
(4) preparing the needle-punched composite microspheres: mixing the obtained reaction liquid and the nano montmorillonite, moving the mixture into a reaction kettle, heating, stirring for reaction, filtering and separating to obtain filter residues, and obtaining the needle-punched composite microspheres;
(5) preparing a self-made waterproof anti-aging coating: weighing thermosetting acrylic resin, needle-punched composite microspheres, isopropanol, propylene glycol monolaurate and ethanol solution, adding into a colloid mill, grinding, mixing and discharging to obtain the self-made waterproof anti-aging coating;
(6) preparing a hydrophobic anti-aging glass film: and (3) coating the self-made waterproof anti-aging coating on the surface of the pretreated glass film by using a coating machine, transferring the coated glass film into an oven after coating, and discharging the glass film after thermocuring to obtain the hydrophobic anti-aging glass film.
Further, the preparation method comprises the following specific steps:
(1) preparing modified titanium sol: mixing titanium isopropoxide and butanol according to the mass ratio of 1:10, placing the mixture into an ultrasonic disperser, performing ultrasonic dispersion for 30-40 min at the frequency of 25-35 kHz to obtain a precursor solution, adding a nitric acid solution with the concentration of 0.1mol/L and deionized water with the concentration of 10 times of the mass of the precursor solution, which are 2 times of the mass of the precursor solution, into the precursor solution, transferring the precursor solution into a water bath kettle at the temperature of 60-80 ℃, stirring and hydrolyzing for 1-3 h to obtain titanium sol, and mixing the obtained titanium sol and trimethylchlorosilane according to the mass ratio of 30:1 to obtain modified titanium sol;
(2) preparation of a pretreated glass film: immersing glass to be treated into the modified titanium sol, standing for 3-5 min, vertically lifting the glass upwards at the speed of 0.5cm/s, immediately placing the glass into a muffle furnace after each layer of film is lifted in an immersion manner, carrying out heat treatment at the temperature of 400-500 ℃ for 10-15 min, and repeating for 5 times to obtain a pretreated glass film;
(3) preparation of reaction solution: mixing 25% sodium silicate solution and 0.5mol/L phosphoric acid solution according to the mass ratio of 6:1 to obtain mixed solution, putting the mixed solution into an ultrasonic oscillator, and carrying out ultrasonic oscillation reaction for 30-40 min at the frequency of 25-35 kHz to obtain reaction solution;
(4) preparing the needle-punched composite microspheres: mixing the obtained reaction liquid and the nano montmorillonite according to the mass ratio of 30:1, then moving the mixture into a reaction kettle, heating the mixture to 200-300 ℃, stirring the mixture at the rotating speed of 200-300 r/min for reaction for 1-2 hours, and then filtering and separating the mixture to obtain filter residues, namely the needle-punched composite microspheres;
(5) preparing a self-made waterproof anti-aging coating: weighing 35-45 parts of thermosetting acrylic resin, 15-20 parts of the needle-punched composite microspheres, 15-20 parts of isopropanol, 3-5 parts of propylene glycol monolaurate and 30-40 parts of 75% ethanol solution by mass, adding into a colloid mill, grinding and mixing for 20-30 min, and discharging to obtain the self-made waterproof anti-aging coating;
(6) preparing a hydrophobic anti-aging glass film: coating machine for the obtained self-made waterproof anti-aging coating is used for coating at the concentration of 3-5 g/cm2The coating amount is coated on the surface of the pretreated glass film, the glass film is moved into an oven after coating is finished, and the glass film is discharged after thermocuring is carried out for 20-30 min at 120-150 ℃, so that the hydrophobic anti-aging glass film can be obtained.
By the scheme, the invention at least has the following advantages:
(1) the invention firstly takes titanium isopropoxide as a raw material, the titanium isopropoxide reacts with acid for hydrolysis to prepare nano titanium sol, the nano titanium sol is modified by trimethylchlorosilane to obtain modified titanium sol, the modified titanium sol forms a pretreated glass film after leaching heat treatment, then sodium silicate and phosphoric acid react to generate an orthosilicic acid reaction solution, nano montmorillonite is added into the orthosilicic acid reaction solution and is heated and hydrolyzed to prepare needle-punched composite microspheres, the needle-punched composite microspheres, thermosetting acrylic resin and other raw materials are blended to prepare a self-made waterproof anti-aging coating, the coating is coated on the surface of a pretreated glass membrane and is thermally cured, and finally the hydrophobic anti-aging glass membrane is prepared.3After the group substitution, the hydrophobic angle is increased from 40 degrees to 120 degrees, the surface of the pretreated glass film is loose, the pretreated glass film has an obvious pore structure, the size of the pore is several to more than ten nanometers, the pore structure undoubtedly increases the micro-surface roughness, so that the hydrophobicity of the glass film is improved, the hydrophobicity is enhanced, meanwhile, the main component of the pretreated glass film is nano titanium dioxide, and the nano titanium dioxide has extremely strong ultraviolet absorptivity and excellent oxidation resistance, so that the ageing resistance of the glass film is effectively improved;
(2) in addition, the invention takes nano-montmorillonite as a nucleus body, the nano-montmorillonite is put into ortho-silicic acid reaction liquid, in the process of heating hydrolysis, ortho-silicic acid is hydrolyzed to generate nano-silica particles, the generated nano-silica particles are adsorbed and fixed by hydroxyl on the surface of the nano-montmorillonite and finally deposited on the surface of the nano-montmorillonite to form needle-punched montmorillonite/silica composite microspheres, the composite microspheres, thermosetting acrylic resin and other raw materials are mixed and coated on the surface of a pretreated glass membrane, after thermocuring, the needle-punched composite microspheres are separated out and uniformly distributed on the surface of the glass to form SiO with meteorite crater-shaped structure2Super hydrophobic membrane, because needle-like structure and meteorite crater structure are storedAnd a rough microscopic surface can be formed by more air, and the contact angle between the surface of the glass film and water drops is increased, so that the hydrophobicity is obviously improved again, and the method has a wide application prospect.
The foregoing is a summary of the present invention, and in order to provide a clear understanding of the technical means of the present invention and to be implemented in accordance with the present specification, the following is a detailed description of the preferred embodiments of the present invention.
Detailed Description
Mixing titanium isopropoxide and butanol according to the mass ratio of 1:10, placing the mixture into an ultrasonic disperser, ultrasonically dispersing the mixture for 30-40 min at the frequency of 25-35 kHz to obtain precursor liquid, adding nitric acid solution with the concentration of 0.1mol/L and deionized water with the mass of 10 times of the precursor liquid, wherein the mass of the nitric acid solution is 2 times of the mass of the precursor liquid, and transferring the mixture into a water bath kettle with the temperature of 60-80 ℃, stirring and hydrolyzing the mixture for 1-3 h to obtain titanium sol for later use; mixing the obtained titanium sol and trimethylchlorosilane according to the mass ratio of 30:1 to obtain modified titanium sol, immersing glass to be treated into the modified titanium sol, standing for 3-5 min, vertically and upwards lifting the glass at the speed of 0.5cm/s, immediately putting the glass into a muffle furnace after each time of dipping and lifting one layer of film, carrying out heat treatment at the temperature of 400-500 ℃ for 10-15 min, and repeating for 5 times to obtain a pretreated glass film; mixing 25% sodium silicate solution and 0.5mol/L phosphoric acid solution according to the mass ratio of 6:1 to obtain mixed solution, putting the mixed solution into an ultrasonic oscillator, and carrying out ultrasonic oscillation reaction for 30-40 min at the frequency of 25-35 kHz to obtain reaction solution; mixing the obtained reaction liquid and the nano montmorillonite according to the mass ratio of 30:1, then moving the mixture into a reaction kettle, heating the mixture to 200-300 ℃, stirring the mixture at the rotating speed of 200-300 r/min for reaction for 1-2 hours, and then filtering and separating the mixture to obtain filter residues, namely the needle-punched composite microspheres; weighing 35-45 parts of thermosetting acrylic resin, 15-20 parts of the needle-punched composite microspheres, 15-20 parts of isopropanol, 3-5 parts of propylene glycol monolaurate and 30-40 parts of 75% ethanol solution by mass, adding into a colloid mill, grinding and mixing for 20-30 min, and discharging to obtain the self-made waterproof anti-aging coating; coating machine for the obtained self-made waterproof anti-aging coating is used for coating at the concentration of 3-5 g/cm2The coating amount of (A) is coated on the pretreated glassAnd (3) moving the glass film surface into an oven after coating, performing thermocuring at 120-150 ℃ for 20-30 min, and discharging to obtain the hydrophobic anti-aging glass film.
Example 1
Mixing titanium isopropoxide and butanol according to the mass ratio of 1:10, placing the mixture into an ultrasonic disperser, performing ultrasonic dispersion for 30min at the frequency of 25kHz to obtain precursor liquid, adding nitric acid solution with the concentration of 0.1mol/L and the mass of deionized water with the mass of 10 times of the mass of the precursor liquid, which are 2 times of the mass of the precursor liquid, into the precursor liquid, moving the precursor liquid into a 60 ℃ water bath kettle, stirring and hydrolyzing for 1h to obtain titanium sol for later use; mixing the obtained titanium sol and trimethylchlorosilane according to the mass ratio of 30:1 to obtain modified titanium sol, immersing glass to be treated into the modified titanium sol, standing for 3min, vertically lifting the glass upwards at the speed of 0.5cm/s, immediately placing the glass into a muffle furnace after each immersion lifting of one film, carrying out heat treatment at the temperature of 400 ℃ for 10min, and repeating for 5 times to obtain a pretreated glass film; mixing 25 mass percent of sodium silicate solution and 0.5mol/L phosphoric acid solution according to the mass ratio of 6:1 to obtain mixed solution, putting the mixed solution into an ultrasonic oscillator, and carrying out ultrasonic oscillation reaction for 30min at the frequency of 25kHz to obtain reaction liquid; mixing the obtained reaction liquid and the nano montmorillonite according to the mass ratio of 30:1, transferring the mixture into a reaction kettle, heating the mixture to 200 ℃, stirring the mixture at the rotating speed of 200r/min for reaction for 1 hour, and filtering and separating the mixture to obtain filter residues, namely the needle-punched composite microspheres; weighing 35 parts of thermosetting acrylic resin, 15 parts of the needle-punched composite microspheres, 15 parts of isopropanol, 3 parts of propylene glycol monolaurate and 30 parts of 75% ethanol solution by mass, adding into a colloid mill, grinding and mixing for 20min, and discharging to obtain the self-made waterproof anti-aging coating; coating machine for the self-made waterproof anti-aging coating obtained by the method is used for coating at the concentration of 3g/cm2The coating amount is coated on the surface of the pretreated glass film, the glass film is moved into an oven after coating is finished, and the glass film is discharged after thermal curing is carried out for 20min at 120 ℃, so that the hydrophobic aging-resistant glass film can be obtained.
Example 2
Mixing titanium isopropoxide and butanol according to the mass ratio of 1:10, placing the mixture into an ultrasonic disperser, performing ultrasonic dispersion for 35min at the frequency of 30kHz to obtain precursor liquid, and adding the precursor liquid with the concentration of 0.1 times of the mass of the precursor liquid by 2 timesmoving the mol/L nitric acid solution and deionized water with the mass of 10 times of that of the precursor solution into a 70 ℃ water bath, stirring and hydrolyzing for 2h to obtain titanium sol for later use; mixing the obtained titanium sol and trimethylchlorosilane according to the mass ratio of 30:1 to obtain modified titanium sol, immersing glass to be treated into the modified titanium sol, standing for 4min, vertically lifting the glass upwards at the speed of 0.5cm/s, immediately placing the glass into a muffle furnace after each immersion lifting of one film, carrying out heat treatment at the temperature of 450 ℃ for 13 min, and repeating for 5 times to obtain a pretreated glass film; mixing 25 mass percent of sodium silicate solution and 0.5mol/L phosphoric acid solution according to the mass ratio of 6:1 to obtain mixed solution, putting the mixed solution into an ultrasonic oscillator, and carrying out ultrasonic oscillation reaction for 35min at the frequency of 30kHz to obtain reaction liquid; mixing the obtained reaction liquid and the nano montmorillonite according to the mass ratio of 30:1, transferring the mixture into a reaction kettle, heating the mixture to 250 ℃, stirring the mixture at the rotating speed of 250r/min for reaction for 2 hours, and filtering and separating the mixture to obtain filter residues, namely the needle-punched composite microspheres; weighing 40 parts of thermosetting acrylic resin, 18 parts of the needle-punched composite microspheres, 18 parts of isopropanol, 4 parts of propylene glycol monolaurate and 35 parts of 75% ethanol solution by mass, adding into a colloid mill, grinding and mixing for 25min, and discharging to obtain the self-made waterproof anti-aging coating; coating machine for the self-made waterproof anti-aging coating obtained by the method is used for coating at the concentration of 4g/cm2The coating amount is coated on the surface of the pretreated glass film, the glass film is moved into an oven after coating is finished, and the glass film is discharged after thermocuring is carried out for 25min at 135 ℃, so that the hydrophobic aging-resistant glass film can be obtained.
Example 3
Mixing titanium isopropoxide and butanol according to the mass ratio of 1:10, placing the mixture into an ultrasonic disperser, performing ultrasonic dispersion for 40min at the frequency of 35kHz to obtain precursor liquid, adding nitric acid solution with the concentration of 0.1mol/L and the mass of deionized water with the mass of 10 times of the mass of the precursor liquid, which are 2 times of the mass of the precursor liquid, into the precursor liquid, moving the precursor liquid into a water bath kettle at the temperature of 80 ℃, stirring and hydrolyzing for 3h to obtain titanium sol for later use; mixing the obtained titanium sol and trimethylchlorosilane according to the mass ratio of 30:1 to obtain modified titanium sol, immersing glass to be treated into the modified titanium sol, standing for 5min, vertically lifting the glass upwards at the speed of 0.5cm/s, immediately placing the glass into a muffle furnace after dipping and lifting one film at the temperature of 500 DEG CHeat treatment is carried out for 15 min at the temperature of (1), and the process is repeated for 5 times to obtain a pretreated glass film; mixing 25 mass percent of sodium silicate solution and 0.5mol/L phosphoric acid solution according to the mass ratio of 6:1 to obtain mixed solution, putting the mixed solution into an ultrasonic oscillator, and carrying out ultrasonic oscillation reaction for 40min at the frequency of 35kHz to obtain reaction liquid; mixing the obtained reaction liquid and the nano montmorillonite according to the mass ratio of 30:1, transferring the mixture into a reaction kettle, heating the mixture to 300 ℃, stirring the mixture at the rotating speed of 300r/min for reaction for 2 hours, and filtering and separating the mixture to obtain filter residues, namely the needle-punched composite microspheres; weighing 45 parts of thermosetting acrylic resin, 20 parts of the needle-punched composite microspheres, 20 parts of isopropanol, 5 parts of propylene glycol monolaurate and 40 parts of 75% ethanol solution by mass, adding into a colloid mill, grinding and mixing for 30min, and discharging to obtain the self-made waterproof anti-aging coating; coating the obtained self-made waterproof anti-aging coating by a coating machine at the ratio of 5g/cm2The coating amount is coated on the surface of the pretreated glass film, the glass film is moved into an oven after coating is finished, and the glass film is discharged after thermal curing is carried out for 30min at 150 ℃, so that the hydrophobic aging-resistant glass film can be obtained.
Comparative example 1: the production method was substantially the same as in inventive example 1, except that the glass surface was not treated to produce the pretreated glass film of the present invention;
comparative example 2: the preparation method was substantially the same as in example 1 of the present invention, except that ordinary silica was used in place of the needle-punched composite microspheres of the present invention;
the examples 1 to 3 of the present invention and the comparative examples 1 to 2 were subjected to the performance test, and the test results are shown in Table 1:
the detection method comprises the following steps:
and (3) detecting the aging resistance: detecting the ultraviolet absorptivity of the glass film, wherein the higher the absorptivity is, the higher the ultraviolet resistance is, and the better the oxidation resistance is;
and (3) detecting hydrophobicity: detecting the contact angle of the surface of the glass film by using a contact angle measuring instrument;
TABLE 1 Performance test results
| Detecting items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Contact angle (°) | 135 | 138 | 140 | 92 | 86 |
| Ultraviolet absorptivity (%) | 85 | 87 | 88 | 10 | 70 |
As can be seen from the detection data in the above table, in comparative example 1 of the present invention, since the pretreated glass film of the present invention was not prepared, both the contact angle and the ultraviolet absorption rate were significantly reduced, and both the hydrophobicity and the aging resistance were significantly reduced, it can be seen that the pretreated glass film of the present invention indeed improves the hydrophobicity and the aging resistance of the glass film;
in comparative example 2, since the needle-punched composite microspheres of the present invention were not used, the contact angle was significantly reduced, the hydrophobicity was significantly reduced, the ultraviolet absorption rate was slightly reduced, and the aging resistance was slightly reduced, which shows that the needle-punched composite microspheres of the present invention certainly improve the hydrophobicity of the glass film of the present invention, and have a wide application prospect.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (4)
1. The hydrophobic anti-aging glass film is prepared by coating a self-made waterproof anti-aging coating on the surface of a pretreated glass film and then thermally curing the coating, and is characterized in that:
the pretreated glass film is prepared by dipping, lifting and heat treatment of modified titanium sol;
the modified titanium sol is prepared by reacting titanium isopropoxide, butanol, a nitric acid solution, deionized water and trimethylchlorosilane;
the self-made waterproof anti-aging coating is prepared by reacting thermosetting acrylic resin, needle-punched composite microspheres, isopropanol, propylene glycol monolaurate and an ethanol solution;
the needle-punched composite microspheres are prepared by reacting reaction liquid with nano montmorillonite;
the reaction solution is prepared by reacting a sodium silicate solution with a phosphoric acid solution.
2. The preparation method of the hydrophobic anti-aging glass film is characterized by comprising the following specific preparation steps:
(1) preparing modified titanium sol: mixing titanium isopropoxide and butanol, performing ultrasonic dispersion, adding a nitric acid solution and deionized water, hydrolyzing to obtain a titanium sol, and mixing the titanium sol and trimethylchlorosilane to obtain a modified titanium sol;
(2) preparation of a pretreated glass film: immersing glass to be treated into the modified titanium sol, standing, lifting, performing heat treatment after each film is immersed and pulled for 5 times to obtain a pretreated glass film;
(3) preparation of reaction solution: mixing a sodium silicate solution and a phosphoric acid solution, and carrying out ultrasonic oscillation reaction to obtain a reaction solution;
(4) preparing the needle-punched composite microspheres: mixing the reaction liquid with the nano montmorillonite, heating and stirring for reaction to obtain the needle-punched composite microspheres;
(5) preparing a self-made waterproof anti-aging coating: weighing thermosetting acrylic resin, needle-punched composite microspheres, isopropanol, propylene glycol monolaurate and ethanol solution, grinding, mixing and discharging to obtain the self-made waterproof anti-aging coating;
(6) preparing a hydrophobic anti-aging glass film: and (3) coating the self-made waterproof anti-aging coating on the surface of the pretreated glass film, and performing thermocuring to obtain the hydrophobic anti-aging glass film.
3. The method for preparing a hydrophobic aging-resistant glass film as claimed in claim 2, characterized by comprising the following specific preparation steps:
(1) preparing modified titanium sol: mixing titanium isopropoxide and butanol, placing the mixture into an ultrasonic disperser for ultrasonic dispersion to obtain a precursor solution, adding a nitric acid solution and deionized water into the precursor solution, transferring the precursor solution into a water bath, stirring and hydrolyzing to obtain titanium sol, and mixing the obtained titanium sol and trimethylchlorosilane to obtain modified titanium sol;
(2) preparation of a pretreated glass film: immersing glass to be treated in the modified titanium sol, standing, vertically lifting the glass upwards, immediately placing the glass in a muffle furnace after each immersion lifting of one layer of film, performing heat treatment, and repeating for 5 times to obtain a pretreated glass film;
(3) preparation of reaction solution: mixing a sodium silicate solution and a phosphoric acid solution to obtain a mixed solution, loading the mixed solution into an ultrasonic oscillator, and carrying out ultrasonic oscillation reaction to obtain a reaction solution;
(4) preparing the needle-punched composite microspheres: mixing the obtained reaction liquid and the nano montmorillonite, moving the mixture into a reaction kettle, heating, stirring for reaction, filtering and separating to obtain filter residues, and obtaining the needle-punched composite microspheres;
(5) preparing a self-made waterproof anti-aging coating: weighing thermosetting acrylic resin, needle-punched composite microspheres, isopropanol, propylene glycol monolaurate and ethanol solution, adding into a colloid mill, grinding, mixing and discharging to obtain the self-made waterproof anti-aging coating;
(6) preparing a hydrophobic anti-aging glass film: and (3) coating the self-made waterproof anti-aging coating on the surface of the pretreated glass film by using a coating machine, transferring the coated glass film into an oven after coating, and discharging the glass film after thermocuring to obtain the hydrophobic anti-aging glass film.
4. The method for preparing a hydrophobic aging-resistant glass film as claimed in claim 2 or 3, characterized by comprising the following specific preparation steps:
(1) preparing modified titanium sol: mixing titanium isopropoxide and butanol according to the mass ratio of 1:10, placing the mixture into an ultrasonic disperser, performing ultrasonic dispersion for 30-40 min at the frequency of 25-35 kHz to obtain a precursor solution, adding a nitric acid solution with the concentration of 0.1mol/L and deionized water with the concentration of 10 times of the mass of the precursor solution, which are 2 times of the mass of the precursor solution, into the precursor solution, transferring the precursor solution into a water bath kettle at the temperature of 60-80 ℃, stirring and hydrolyzing for 1-3 h to obtain titanium sol, and mixing the obtained titanium sol and trimethylchlorosilane according to the mass ratio of 30:1 to obtain modified titanium sol;
(2) preparation of a pretreated glass film: immersing glass to be treated into the modified titanium sol, standing for 3-5 min, vertically lifting the glass upwards at the speed of 0.5cm/s, immediately placing the glass into a muffle furnace after each layer of film is lifted in an immersion manner, carrying out heat treatment at the temperature of 400-500 ℃ for 10-15 min, and repeating for 5 times to obtain a pretreated glass film;
(3) preparation of reaction solution: mixing 25% sodium silicate solution and 0.5mol/L phosphoric acid solution according to the mass ratio of 6:1 to obtain mixed solution, putting the mixed solution into an ultrasonic oscillator, and carrying out ultrasonic oscillation reaction for 30-40 min at the frequency of 25-35 kHz to obtain reaction solution;
(4) preparing the needle-punched composite microspheres: mixing the obtained reaction liquid and the nano montmorillonite according to the mass ratio of 30:1, then moving the mixture into a reaction kettle, heating the mixture to 200-300 ℃, stirring the mixture at the rotating speed of 200-300 r/min for reaction for 1-2 hours, and then filtering and separating the mixture to obtain filter residues, namely the needle-punched composite microspheres;
(5) preparing a self-made waterproof anti-aging coating: weighing 35-45 parts of thermosetting acrylic resin, 15-20 parts of the needle-punched composite microspheres, 15-20 parts of isopropanol, 3-5 parts of propylene glycol monolaurate and 30-40 parts of 75% ethanol solution by mass, adding into a colloid mill, grinding and mixing for 20-30 min, and discharging to obtain the self-made waterproof anti-aging coating;
(6) preparing a hydrophobic anti-aging glass film: coating machine for the obtained self-made waterproof anti-aging coating is used for coating at the concentration of 3-5 g/cm2The coating amount is coated on the surface of the pretreated glass film, the glass film is moved into an oven after coating is finished, and the glass film is discharged after thermocuring is carried out for 20-30 min at 120-150 ℃, so that the glass film is obtainedTo hydrophobic aging-resistant glass films.
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| CN112226771A (en) * | 2020-09-28 | 2021-01-15 | 长安大学 | Super-hydrophobic composite film layer of titanium alloy and preparation method thereof |
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