CN111606574A - Glycosyl super-hydrophilic modified antifogging glass and preparation method and application thereof - Google Patents
Glycosyl super-hydrophilic modified antifogging glass and preparation method and application thereof Download PDFInfo
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- CN111606574A CN111606574A CN202010530451.1A CN202010530451A CN111606574A CN 111606574 A CN111606574 A CN 111606574A CN 202010530451 A CN202010530451 A CN 202010530451A CN 111606574 A CN111606574 A CN 111606574A
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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
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
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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
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3405—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of organic materials
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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
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
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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
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
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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
- C03C2218/32—After-treatment
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- Surface Treatment Of Glass (AREA)
Abstract
The invention discloses glycosyl super-hydrophilic modified antifogging glass and a preparation method and application thereof, wherein the surface of the glass is subjected to hydroxylation treatment, and the hydroxylated glass is coupled with saccharides through a silanization reagent, the glycosyl and the surface of the glass are connected through the silanization reagent, so that the connectivity between glycosyl and the surface of the glass can be enhanced, the adhesive force and the mechanical strength are enhanced, the flexible connection effect of the silanization reagent can be used as a buffer structure between a glycosyl hydrophilic layer and the glass, the larger surface tension generated after the glycosyl hydrophilic layer is contacted with water is relieved, the hydrophilic effect is enhanced, the successfully modified glass surface contact angle is less than 10 degrees, and the glycosyl super-hydrophilic modified antifogging glass has excellent light transmittance and better antifogging and antifreezing effects. In addition, the hydrophilic coating is obtained in a chemical bond modification mode instead of a coating mode, so that the obtained glass has a self-cleaning function.
Description
Technical Field
The invention relates to glycosyl super-hydrophilic modified antifogging glass and a preparation method and application thereof, belonging to the technical field of functional material preparation.
Background
Transparent materials such as glass, quartz and the like have wide application in daily life, industry, agriculture and medical treatment, such as mirrors, various medical endoscope lenses, automobile windshields and the like, and the application of the materials facilitates the life of people. However, when the humidity is high or the temperature is low, the surface of these materials is easily atomized, that is, moisture or steam is condensed on the surface of the materials to form tiny water drops, thereby affecting the sight line and bringing about a lot of inconvenience and even causing disasters.
At present, a great deal of extensive research on the anti-fog technology has been carried out, and a great variety of anti-fog methods are also obtained, and generally divided into the following methods: directly coating substances such as a surfactant and the like on a transparent material; doping a surfactant in the manufacturing process of the transparent material; and thirdly, coating a polymer film on the surface of the transparent material.
The method (i) mainly uses a hydrophilic coating. The surface tension of the glass product is improved by using the hydrophilic coating, so that fog spreads and wets on the surface of the glass product, and fog drops on the surface of the glass are converted into a uniform water film, thereby avoiding the generation of the fog. The hydrophilic coating is usually applied to two types of substances, one is that inorganic hydrophilic fillers such as silicon dioxide, titanium dioxide and the like have the advantages of high hardness and wear resistance, but the practical application of the hydrophilic coating is influenced because the surface polar groups of the inorganic hydrophilic fillers are limited and the other one needs special ultraviolet illumination conditions and the like; the other is organic hydrophilic polymer, which usually has hydrophilic polar groups such as carboxyl, hydroxyl, amino and the like, and the polymer has good film forming property, but has limited capabilities of hardness, wear resistance and the like. Therefore, a great deal of literature patents are directed to the preparation of antifogging coatings by combining inorganic and organic means, and this is also considered to be the hydrophilic coating which is most likely to achieve a long-term antifogging function so far.
And the conventional surfactant is generally used in the method (ii). By introducing the surfactant into the surface needing antifogging and utilizing the property of reducing the surface tension of water when the surfactant is contacted with the fog drops, the fog forms a layer of uniform water film instead of the fog drops, thereby avoiding the influence of the fog on the optical transparency of the glass. However, the surfactant can be gradually lost along with the contact of fog, so that the service life of the surfactant is short, and the antifogging capability of the glass surface can be quickly lost.
Compared with the two methods, the method has better antifogging effect, longer efficacy, better mechanical property and more wear resistance.
Currently, the antifogging effect and durability of these techniques are not yet satisfactory. The research finds that the main reasons for the short aging of the existing hydrophilic anti-fog technology or product include the following aspects: (1) hydrophilic surfaces tend to cause impurities such as dust in the environment to adsorb on their surfaces, on the one hand due to their high surface energy and on the other hand due to the action of surface static electricity, resulting in loss of surface anti-fogging ability: (2) after the hydrophilic polymer in the hydrophilic coating is subjected to antifogging use for several times, partial molecules are dissolved or swelled, or microorganisms such as bacteria in the environment grow and enrich on the surface, so that the surface structure is damaged to reduce or lose the antifogging capability; (3) the hydrophobic chain segment of the polymer in the hydrophilic coating migrates to the surface along with the time, and the surface tension of the coating is reduced, so that the duration of the antifogging capability is not long; (4) the coating has insufficient adhesion on the glass substrate or insufficient mechanical strength, so that the coating is damaged by slight external force during use, and the antifogging capability is lost.
Therefore, the development and development of coatings with long-acting antifogging function are the development direction of the existing antifogging technology, and the research and development of novel self-cleaning antifogging glass which is convenient, good in wear resistance and weather resistance and low in cost is necessary and meaningful. Namely, the antifogging surface modification with simple preparation method, low raw material cost, excellent wear resistance, cohesiveness, transparency and durability is the main research direction of hydrophilic antifogging technology at home and abroad at present.
Aiming at the reasons and conforming to the development trend of the times, the invention integrates the factors of raw materials, processes and the like, adopts a new technical means to improve the anti-fog durability of the anti-fog coating and meets the requirement of practical application.
Disclosure of Invention
In order to solve the technical problems, the hydroxylated glass is coupled with saccharides through a silylation reagent by hydroxylating the surface of the glass, and the contact angle of the successfully modified glass surface is less than 10 degrees (the contact angle is less than 10 degrees, namely the super-hydrophilic surface), so that the glass has excellent light transmittance, better anti-fog and anti-freezing effects and self-cleaning function. The glass successfully modified by the invention can be used for glass products needing self-cleaning, antifogging and antifreezing performance and permeability.
The first purpose of the invention is to provide sugar-based super-hydrophilic modified antifogging glass, which comprises a glass substrate layer and a sugar-based hydrophilic layer, and is obtained by connecting a glass substrate with a sugar substance through a silylation agent after hydroxylation treatment.
Further, the saccharide substance is reducing sugar or reducing sugar lactone.
Further, the reducing sugar is one or more of glucose, lactose, maltose, fructose and galactose.
Further, the silylation reagent is a silylation reagent A or a silylation reagent B, the structural formula of the silylation reagent A is shown in (1), and the structural formula of the silylation reagent B is shown in (2):
further, the molar ratio of the saccharide to the silylation reagent is 1: 0.5-5.
The second purpose of the invention is to provide a preparation method of the sugar-based super-hydrophilic modified antifogging glass, which comprises the following steps:
s1, ultrasonically cleaning the glass substrate in absolute ethyl alcohol, and drying for later use;
s2, placing the glass substrate cleaned in the S1 step in H2O2︰NH3·H2O︰H2Soaking in a solution with the volume ratio of O being (1-3): 3-8, and cleaning after soaking;
s3, placing the glass substrate cleaned in the S2 step in H2O2︰H2SO4Soaking in a solution with a volume ratio of (2-7): 3-8, heating in a water bath at 30-90 ℃, washing with absolute ethyl alcohol, and drying for later use to obtain hydroxylated glass;
and S4, dissolving the saccharides in the solvent, adding a silanization reagent and hydroxylated glass, reacting for 2-72 h, and washing and drying to obtain the glycosyl-based super-hydrophilic modified antifogging glass.
Further, the solvent of the saccharide is methanol.
Further, the water bath heating time is 1-8 h.
Furthermore, the time of the ultrasonic treatment is 10-120 minutes.
The third purpose of the invention is to provide the application of the sugar-based super-hydrophilic modified anti-fog glass.
The invention has the beneficial effects that:
according to the invention, the glass surface is subjected to hydroxylation treatment, the hydroxylated glass is coupled with saccharides through a silanization reagent, the saccharide base is connected with the glass surface through the silanization reagent, the connectivity between the saccharide base and the glass surface can be enhanced, the adhesive force and the mechanical strength are enhanced, the flexible connection effect of the silanization reagent can be utilized, the saccharide base hydrophilic layer can be used as a buffer structure in front of the saccharide base hydrophilic layer and the glass, the larger surface tension generated after the saccharide base hydrophilic layer is contacted with water is relieved, the hydrophilic effect is enhanced, the contact angle of the successfully modified glass surface is less than 10 degrees, and the glass surface has excellent light transmittance and better antifogging and antifreezing effects. In addition, the hydrophilic coating is obtained in a chemical bond modification mode instead of a coating mode, so that the obtained glass has a self-cleaning function.
The solvent used in the invention comprises water, methanol, ethanol, ammonia water, hydrogen peroxide and concentrated sulfuric acid, and no other volatile toxic harmful organic solvent is used. The method has the advantages of wide sources of reaction raw materials, low price, no toxicity, no harm, mild conditions in the preparation process, simple and convenient operation, low content of organic matters in the reaction waste liquid, small environmental pollution, greenness and environmental protection, and is suitable for industrial mass production.
Drawings
FIG. 1 is a test chart of water contact angle of super hydrophilic glass surface;
FIG. 2 shows the antifogging effect of super-hydrophilic glass.
Detailed Description
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
Example 1:
and washing the glass sheet, and drying for later use. Adding 30mL of chemically pure absolute ethyl alcohol (washing) into a beaker, putting the glass sheets into the beaker, performing ultrasonic treatment for 30min, washing with water, and drying for later use; placing the glass sheet in a volume ratio of H2O2︰NH3·H2O︰H2Soaking in solution (V/V/V) at ratio of O3: 5(36ml,36ml,60ml) for 30min, and washing with water; placing the glass sheet and glass ball in H2O2︰H2SO4Soaking at ratio of 4: 6(32ml,48ml) (V/V) (solution heating), heating in water bath at 90 deg.C for 1h, washing with water, washing with anhydrous ethanol, and blow-drying to obtain hydroxylated glass sheet.
10mmol of glucose was dissolved in methanol, and the solution was heated to dissolve it to be transparent, and 15mmol of silylating agent A and the above-obtained hydroxylated glass plate were added thereto and stirred at room temperature for 48 hours. Washing with water, washing with ethanol, and drying to obtain the successfully modified super-hydrophilic glass surface.
Example 2:
and washing the glass sheet, and drying for later use. Adding 30mL of chemically pure absolute ethanol to the beaker (Wash)Washing), placing the glass sheet in the ultrasonic wave generator, performing ultrasonic treatment for 40min, washing with water, and drying for later use; placing the glass sheet in a volume ratio of H2O2︰NH3·H2O︰H2Soaking in O1: 3(12ml,12ml,36ml) (V/V/V) for 30min, and washing with water; placing the glass sheet and glass ball in H2O2︰H2SO4Soaking at ratio of 4: 5(32ml,40ml) (V/V) (solution heating), heating in water bath at 50 deg.C for 2 hr, washing with water, washing with anhydrous ethanol, and blow-drying to obtain hydroxylated glass sheet.
Dissolving 10mmol of gluconolactone in methanol, heating to dissolve to be transparent, adding 10mmol of silylation reagent A and the hydroxylated glass sheet, and stirring at room temperature for 36 h. Washing with water, washing with ethanol, and drying to obtain the successfully modified super-hydrophilic glass surface.
Example 3:
and washing the glass sheet, and drying for later use. Adding 30mL of chemically pure absolute ethyl alcohol (washing) into a beaker, putting glass sheets into the beaker, performing ultrasonic treatment for 40min, washing with water, and drying for later use; placing the glass sheet in a volume ratio of H2O2︰NH3·H2O︰H2Soaking in O1: 3(12ml,12ml,36ml) (V/V/V) for 30min, and washing with water; placing the glass sheet and glass ball in H2O2︰H2SO4Soaking at ratio of 4: 5(32ml,40ml) (V/V) (solution heating), heating in water bath at 50 deg.C for 2 hr, washing with water, washing with anhydrous ethanol, and blow-drying to obtain hydroxylated glass sheet.
Dissolving 10mmol of gluconolactone in methanol, heating to dissolve to be transparent, adding 10mmol of silylation reagent B and the hydroxylated glass sheet, and stirring at room temperature for 36 h. Washing with water, washing with ethanol, and drying to obtain the successfully modified super-hydrophilic glass surface.
Example 4:
and washing the glass sheet, and drying for later use. Adding 30mL of chemically pure absolute ethyl alcohol (washing) into a beaker, putting glass sheets into the beaker, performing ultrasonic treatment for 40min, washing with water, and drying for later use; placing the glass sheet in a volume ratio of H2O2︰NH3·H2O︰H2Soaking in O1: 3(12ml,12ml,36ml) (V/V/V) for 30min, and washing with water; placing the glass sheet and glass ball in H2O2︰H2SO4Soaking at ratio of 4: 5(32ml,40ml) (V/V) (solution heating), heating in water bath at 50 deg.C for 2 hr, washing with water, washing with anhydrous ethanol, and blow-drying to obtain hydroxylated glass sheet.
15mmol of lactose was dissolved in methanol, heated to be transparent, and 10mmol of silylating agent B and the hydroxylated glass plate prepared above were added thereto, and stirred at room temperature for 40 hours. Washing with water, washing with ethanol, and drying to obtain the successfully modified super-hydrophilic glass surface.
Example 5:
and washing the glass sheet, and drying for later use. Adding 30mL of chemically pure absolute ethyl alcohol (washing) into a beaker, putting a glass sheet into the beaker, performing ultrasonic treatment for 100min, washing with water, and drying for later use; placing the glass sheet in a volume ratio of H2O2︰NH3·H2O︰H2Soaking in water (V/V/V) at ratio of 1: 5(12ml,12ml,60ml) for 30min, and washing with water; placing the glass sheet and glass ball in H2O2︰H2SO4Soaking at ratio of 4: 6(32ml,48ml) (V/V) (solution heating), heating in water bath at 90 deg.C for 8 hr, washing with water, washing with anhydrous ethanol, and blow-drying to obtain hydroxylated glass sheet.
10mmol of lactose is dissolved in methanol and heated to be transparent, 10mmol of silanization reagent B and the hydroxylated glass sheet prepared above are added, and the mixture is stirred for 36 hours at room temperature. Washing with water, washing with ethanol, and drying to obtain the successfully modified super-hydrophilic glass surface.
Example 6:
the hydrophilicity test of the glass prepared in the embodiment 1-5 shows that the glass has a contact angle of less than 10 degrees on the surface of the glass with a super-hydrophilic surface, and has excellent light transmittance and good anti-fogging effect (see fig. 2). The performance test results of the super-hydrophilic surface glass prepared in the embodiment 1-6 are shown in table 1:
TABLE 1
As can be seen from Table 1, the super hydrophilic surface glass of the present invention has both extremely high light transmittance and super hydrophilicity: the light transmittance is higher than 95%, and the contact angle of the glass surface successfully modified by super-hydrophilicity to water in the air is 0-10 degrees. The successfully modified glass of the present invention can be used for glass products requiring antifogging and antifreezing properties and permeability.
And the modified glass surface is exposed in the air and placed for 15 days, and then the contact angle of a water drop is measured, as shown in table 1, the contact angle of the water drop is basically unchanged, which shows that the super-hydrophilic glass surface can be stable for a long time in the air, has excellent antifogging performance and has an excellent self-cleaning function.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. The sugar-based super-hydrophilic modified antifogging glass is characterized by comprising a glass substrate layer and a sugar-based hydrophilic layer, wherein the glass substrate layer is subjected to hydroxylation treatment and then is connected with saccharides through a silylation reagent.
2. The sugar-based superhydrophilic modified anti-fog glass of claim 1, wherein said sugar-based substance is a reducing sugar or said reducing sugar lactone.
3. The sugar-based super-hydrophilic modified antifogging glass according to claim 2, wherein the reducing sugar is one or more of glucose, lactose, maltose, fructose and galactose.
4. The sugar-based superhydrophilic modified antifogging glass of claim 1, wherein said silylation agent is silylation agent a or silylation agent B, said silylation agent a has a structural formula shown in (1), and said silylation agent B has a structural formula shown in (2):
5. the sugar-based super-hydrophilic modified antifogging glass according to claim 1, wherein the molar ratio of the sugar substance to the silylation agent is 1: 0.5-5.
6. The preparation method of the sugar-based super-hydrophilic modified antifogging glass according to any one of claims 1 to 5, characterized by comprising the following steps:
s1, ultrasonically cleaning the glass substrate in absolute ethyl alcohol, and drying for later use;
s2, placing the glass substrate cleaned in the S1 step in H2O2︰NH3·H2O︰H2Soaking in a solution with the volume ratio of O being (1-3): 3-8, and cleaning after soaking;
s3, placing the glass substrate cleaned in the S2 step in H2O2︰H2SO4Soaking in a solution with a volume ratio of (2-7): 3-8, and adding in a water bath at 30-90 DEG CCleaning with hot and absolute ethyl alcohol, and blow-drying for later use to obtain hydroxylated glass;
and S4, dissolving the saccharides in the solvent, adding a silanization reagent and hydroxylated glass, reacting for 2-72 h, and washing and drying to obtain the glycosyl-based super-hydrophilic modified antifogging glass.
7. The method of claim 6, wherein the solvent for the saccharide is methanol.
8. The method according to claim 6, wherein the heating time in the water bath is 1-8 h.
9. The method of claim 6, wherein the time period of the ultrasound is 10 to 120 minutes.
10. Use of the sugar-based superhydrophilic modified anti-fog glass of any one of claims 1-5.
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