阅读说明：本技术 一种高透光隔热玻璃及其制备方法 (High-light-transmittance heat-insulating glass and preparation method thereof ) 是由 华才升 于 2021-08-10 设计创作，主要内容包括：本发明公开了一种高透光隔热玻璃及其制备方法,涉及节能玻璃领域,通过将耐污乳液加入至混合器中,搅拌的条件下依次加入去离子水、成膜助剂、流平剂,加入完毕后继续剪切,之后加入改性隔热纳米粉分散液继续剪切,之后加入消泡剂并搅拌,之后静置、过滤,得到隔热涂料,将隔热涂料均匀涂于清洗过的玻璃基底表面,自然流平,于室温无尘条件下晾干,待表干后,置于烘箱烘烤,再于室温无尘条件下放置,得到该高透光隔热玻璃；该高透光隔热玻璃通过耐污乳液,使得隔热涂层维持高透光性的同时具有自清洁耐污效果,通过改性隔热纳米粉分散液能够使得隔热涂层具有吸收隔热效果,赋予了玻璃良好的隔热性能。(The invention discloses high-light-transmission heat-insulating glass and a preparation method thereof, and relates to the field of energy-saving glass.A stain-resistant emulsion is added into a mixer, deionized water, a film-forming assistant and a leveling agent are sequentially added under the condition of stirring, the shearing is continued after the addition is finished, then a modified heat-insulating nano powder dispersion liquid is added for continuing the shearing, then a defoaming agent is added and the stirring is carried out, the standing and the filtering are carried out to obtain a heat-insulating coating, the heat-insulating coating is uniformly coated on the surface of a cleaned glass substrate, the natural leveling is carried out, the glass substrate is dried in a dust-free condition at room temperature, the glass substrate is placed in an oven for baking after being dried, and the glass substrate is placed in a dust-free condition at room temperature to obtain the high-light-transmission heat-insulating glass; the high-light-transmission heat-insulation glass has the advantages that the stain-resistant emulsion enables the heat-insulation coating to have the self-cleaning stain-resistant effect while maintaining high light transmission, the heat-insulation coating can have the absorption heat-insulation effect through the modified heat-insulation nano powder dispersion liquid, and the glass is endowed with good heat-insulation performance.)

1. The high-light-transmission heat-insulation glass is characterized by comprising a glass substrate and a heat-insulation coating positioned on the upper surface and the lower surface of the glass substrate, wherein the heat-insulation coating is formed by curing a heat-insulation coating;

the heat insulation coating comprises the following components in parts by weight:

100-150 parts of stain-resistant emulsion, 30-50 parts of modified heat-insulating nano powder dispersion liquid, 5-10 parts of film-forming assistant, 0.2-1 part of flatting agent, 0.2-1 part of defoaming agent and 10-30 parts of deionized water;

the high-light-transmission heat-insulation glass is prepared by the following steps:

the method comprises the following steps: adding the stain-resistant emulsion into a mixer, sequentially adding deionized water, a film-forming aid and a flatting agent under the condition that the stirring rate is 400-600r/min, continuing to shear for 20-30min after the addition is finished, then adding the modified heat-insulating nano-powder dispersion liquid, continuing to shear for 1-2h under the condition that the stirring rate is 800-1100r/min, then adding a defoaming agent under the condition that the stirring rate is 100-300r/min, stirring for 10-20min, then standing for 2-3h, and filtering to obtain the heat-insulating coating;

step two: uniformly coating the heat-insulating coating on the surface of a cleaned glass substrate, naturally leveling, airing at room temperature under a dust-free condition, placing in an oven at 70 ℃ for drying for 1h after surface drying, and then placing at room temperature under the dust-free condition for 1-2h to obtain the high-light-transmission heat-insulating glass.

2. The high-light-transmission heat-insulation glass according to claim 1, wherein the film-forming assistant is dodecyl alcohol ester, the leveling agent is a polyurethane leveling agent 2020, and the defoaming agent is a silicone defoaming agent.

3. The high-transparency heat-insulating glass as claimed in claim 1, wherein the anti-fouling emulsion is prepared by the following steps:

a1: adding 1/3 methyl methacrylate, 1/3 n-butyl acrylate and 1/3 hydroxypropyl acrylate into a beaker, stirring and dispersing for 30-40min under the condition of stirring speed of 500-800r/min to obtain prepolymer A, adding the rest of methyl methacrylate, n-butyl acrylate, hydroxypropyl acrylate and dodecafluoroheptyl methacrylate into another beaker, stirring and dispersing for 30-40min under the condition of stirring speed of 500-800r/min to obtain prepolymer B;

a2: adding the prepolymer A and deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring and dropwise adding a potassium persulfate aqueous solution A under the condition that the stirring speed is 300-500r/min, controlling the dropping speed to be 1 drop/s, heating to 50-55 ℃ after the dropping is finished, adding an emulsifier, heating to 80-90 ℃ after the emulsifier is completely dissolved, stirring and reacting for 20-30min to obtain an emulsion;

a3: uniformly mixing the prepolymer B and a potassium persulfate aqueous solution B, then dropwise adding the mixture into the emulsion while stirring, controlling the dropping rate to be 1 s, stirring and reacting for 2-3h at the temperature of 80-85 ℃ after the dropping is finished, then cooling the reaction product to room temperature, adding ammonia water to adjust the pH value to 7, and obtaining the stain-resistant emulsion.

4. The high-transmittance thermal insulation glass according to claim 3, wherein the molar ratio of the methyl methacrylate, the n-butyl acrylate, the hydroxypropyl acrylate and the dodecafluoroheptyl methacrylate in the step A1 is 0.1: 0.08: 0.04: 0.05.

5. the high-light-transmission heat-insulating glass according to claim 3, wherein the prepolymer A, the deionized water, the potassium persulfate aqueous solution A and the emulsifier in the step A2 are used in a ratio of 25 g: 100mL of: 10mL of: 1.2g, wherein the concentration of the potassium persulfate aqueous solution A is 6g/L, and the emulsifier is sodium dodecyl sulfate and dodecyl phenol polyoxyethylene ether according to the mass ratio of 1: 2, or a mixture thereof.

6. The high-transmittance insulating glass according to claim 3, wherein the prepolymer B and the aqueous solution B of potassium persulfate in the step A3 are used in a ratio of 30 g: 100mL, wherein the mass fraction of the ammonia water is 10-15%.

7. The high-light-transmission heat-insulating glass as claimed in claim 1, wherein the modified heat-insulating nano-powder dispersion is prepared by the following steps:

b1: adding acrylic acid and deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant pressure dropping funnel, and stirring at room temperature and a stirring speed of 500-;

b2: adding zinc acetate and gallium nitrate into the acrylic acid solution, continuously stirring for 20-50min, then dropwise adding the ammonium persulfate aqueous solution while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 10-30min after the dropwise adding is finished, and then continuously stirring and reacting for 20-30min under the condition of heating to 100 ℃ and 110 ℃ to obtain a nano powder precursor;

b3: placing the nano powder precursor in a vacuum drying box, drying for 2-3h at the temperature of 230-270 ℃, then taking out, cooling, grinding, then placing in a muffle furnace, and calcining for 3-4h at the temperature of 600-800 ℃ to obtain heat-insulating nano powder;

b4: adding the heat-insulating nano powder and an ethanol aqueous solution into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, and stirring for 30-60min under the condition that the stirring speed is 2000-3000r/min to obtain a heat-insulating nano powder dispersion liquid;

b5: adding a silane coupling agent KH-570 into an ethanol aqueous solution, uniformly stirring, then dropwise adding into the heat-insulating nano powder dispersion liquid while stirring at the temperature of 70-80 ℃ and the stirring speed of 500-800r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring and reacting for 2-3h after the dropwise adding is finished, then performing rotary evaporation, and then performing ultrasonic dispersion for 10-20min under the ultrasonic frequency of 45-65kHz to obtain the modified heat-insulating nano powder dispersion liquid.

8. The high-light-transmission heat-insulating glass according to claim 7, wherein the mass ratio of the acrylic acid to the deionized water in the step B1 is 7: 3; the mass ratio of the zinc acetate solution to the acrylic acid solution in the step B2 is 3: 20, the molar ratio of the zinc acetate to the gallium nitrate is 20-25: 1, the mass fraction of the ammonium persulfate aqueous solution is 2-5%, and the addition amount of the ammonium persulfate is 0.05-0.1 of the weight of acrylic acid.

9. The high-transmittance thermal insulation glass according to claim 7, wherein the ethanol aqueous solution in the step B4 is absolute ethanol, and the ratio of ethanol in the ethanol aqueous solution is 3: 1 is dissolved in deionized water to form a solution, and the dosage ratio of the heat-insulating nano powder to the ethanol water solution is 1 g: 20-50 mL; the dosage ratio of the silane coupling agent KH-570 to the ethanol aqueous solution in the step B5 is 1 g: 10-20mL, wherein the addition amount of the silane coupling agent KH-570 is 1.0-5.0% of the weight of the heat-insulating nano powder.

10. The method for preparing high-light-transmission heat-insulation glass according to claim 1, characterized by comprising the following steps:

the method comprises the following steps: weighing 100 parts of stain-resistant emulsion, 150 parts of modified heat-insulating nano powder dispersion liquid, 30-50 parts of film-forming assistant, 0.2-1 part of flatting agent, 0.2-1 part of defoaming agent and 10-30 parts of deionized water according to parts by weight;

step two: adding the stain-resistant emulsion into a mixer, sequentially adding deionized water, a film-forming aid and a flatting agent under the condition that the stirring rate is 400-600r/min, continuing to shear for 20-30min after the addition is finished, then adding the modified heat-insulating nano-powder dispersion liquid, continuing to shear for 1-2h under the condition that the stirring rate is 800-1100r/min, then adding a defoaming agent under the condition that the stirring rate is 100-300r/min, stirring for 10-20min, then standing for 2-3h, and filtering to obtain the heat-insulating coating;

step three: uniformly coating the heat-insulating coating on the surface of a cleaned glass substrate, naturally leveling, airing at room temperature under a dust-free condition, placing in an oven at 70 ℃ for drying for 1h after surface drying, and then placing at room temperature under the dust-free condition for 1-2h to obtain the high-light-transmission heat-insulating glass.

Technical Field

The invention relates to the field of energy-saving glass, in particular to high-light-transmission heat-insulation glass and a preparation method thereof.

Background

The large-area glass window and the glass curtain wall are widely used in modern buildings and vehicles, the heat radiation of sunlight can increase the utilization rate of an indoor air conditioner in summer, and the indoor heat is easy to dissipate through glass in winter to cause energy waste, so that the development and application research of energy-saving glass is devoted, a novel heat insulation material is developed, the energy consumption is reduced, and the glass window and the glass curtain wall have important practical significance;

solar radiation (including about 3% ultraviolet, 47% visible light and 50% infrared) on the surface of the earth is a main cause for the temperature rise in summer, building doors and windows need to effectively control the solar radiation to meet the requirements of heat preservation and heat insulation, and the existing heat preservation and heat insulation functions of building glass mainly have three ways at present: firstly, hollow glass is adopted; secondly, coating glass; thirdly, transparent heat-insulating functional coating; the hollow glass has good heat preservation performance, but has high requirement on sealing performance and poor heat insulation effect; the coated glass has a certain reflection effect on sunlight, the transmittance of visible light is seriously influenced, and the coating technology has high cost and complex operation and cannot be widely applied;

the latest research shows that the transparent nano composite coating can effectively improve the heat insulation performance of glass, thereby drawing extensive attention of people, and the research finds that the transparent nano heat insulation functional coating has better infrared shielding effect, and the preparation process of the coating is simple, the operation is convenient and the popularization is easy;

therefore, the key point of the invention is to prepare the high-light-transmission heat-insulation glass by using the low-cost heat-insulation coating.

Disclosure of Invention

In order to overcome the technical problems, the invention aims to provide high-light-transmission heat-insulation glass and a preparation method thereof, wherein the high-light-transmission heat-insulation glass comprises the following steps: the stain-resistant emulsion is added into a mixer, deionized water, a film-forming assistant and a flatting agent are sequentially added under the stirring condition, the mixture is continuously sheared after being added, then modified heat-insulating nano powder dispersion liquid is added for continuous shearing, then a defoaming agent is added and the mixture is stirred, then the mixture is stood and filtered to obtain a heat-insulating coating, the heat-insulating coating is uniformly coated on the surface of a cleaned glass substrate, the natural leveling is carried out, the glass substrate is dried in a dust-free condition at room temperature, the dried glass substrate is placed in an oven for baking after being surface dried, and then the glass substrate is placed in the dust-free condition at room temperature to obtain the high-light-transmission heat-insulating glass.

The purpose of the invention can be realized by the following technical scheme:

the high-light-transmission heat-insulating glass comprises a glass substrate and a heat-insulating coating positioned on the upper surface and the lower surface of the glass substrate, wherein the heat-insulating coating is formed by curing a heat-insulating coating;

the heat insulation coating comprises the following components in parts by weight:

100-150 parts of stain-resistant emulsion, 30-50 parts of modified heat-insulating nano powder dispersion liquid, 5-10 parts of film-forming assistant, 0.2-1 part of flatting agent, 0.2-1 part of defoaming agent and 10-30 parts of deionized water;

the high-light-transmission heat-insulation glass is prepared by the following steps:

the method comprises the following steps: adding the stain-resistant emulsion into a mixer, sequentially adding deionized water, a film-forming aid and a flatting agent under the condition that the stirring rate is 400-600r/min, continuing to shear for 20-30min after the addition is finished, then adding the modified heat-insulating nano-powder dispersion liquid, continuing to shear for 1-2h under the condition that the stirring rate is 800-1100r/min, then adding a defoaming agent under the condition that the stirring rate is 100-300r/min, stirring for 10-20min, then standing for 2-3h, and filtering to obtain the heat-insulating coating;

step two: uniformly coating the heat-insulating coating on the surface of a cleaned glass substrate, naturally leveling, airing at room temperature under a dust-free condition, placing in an oven at 70 ℃ for drying for 1h after surface drying, and then placing at room temperature under the dust-free condition for 1-2h to obtain the high-light-transmission heat-insulating glass.

As a further scheme of the invention: the film-forming assistant is dodecyl alcohol ester, the leveling agent is a polyurethane leveling agent 2020, and the defoaming agent is an organic silicon defoaming agent.

As a further scheme of the invention: the preparation process of the stain-resistant emulsion comprises the following steps:

a1: adding 1/3 methyl methacrylate, 1/3 n-butyl acrylate and 1/3 hydroxypropyl acrylate into a beaker, stirring and dispersing for 30-40min under the condition of stirring speed of 500-800r/min to obtain prepolymer A, adding the rest of methyl methacrylate, n-butyl acrylate, hydroxypropyl acrylate and dodecafluoroheptyl methacrylate into another beaker, stirring and dispersing for 30-40min under the condition of stirring speed of 500-800r/min to obtain prepolymer B;

a2: adding the prepolymer A and deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, stirring and dropwise adding a potassium persulfate aqueous solution A under the condition that the stirring speed is 300-500r/min, controlling the dropping speed to be 1 drop/s, heating to 50-55 ℃ after the dropping is finished, adding an emulsifier, heating to 80-90 ℃ after the emulsifier is completely dissolved, stirring and reacting for 20-30min to obtain an emulsion;

a3: uniformly mixing the prepolymer B and a potassium persulfate aqueous solution B, then dropwise adding the mixture into the emulsion while stirring, controlling the dropping rate to be 1 s, stirring and reacting for 2-3h at the temperature of 80-85 ℃ after the dropping is finished, then cooling the reaction product to room temperature, adding ammonia water to adjust the pH value to 7, and obtaining the stain-resistant emulsion.

The reaction principle is as follows:

as a further scheme of the invention: the molar ratio of methyl methacrylate, n-butyl acrylate, hydroxypropyl acrylate, and dodecafluoroheptyl methacrylate in step a1 is 0.1: 0.08: 0.04: 0.05.

as a further scheme of the invention: the using amount ratio of the prepolymer A, the deionized water, the potassium persulfate aqueous solution A and the emulsifier in the step A2 is 25 g: 100mL of: 10mL of: 1.2g, wherein the concentration of the potassium persulfate aqueous solution A is 6g/L, and the emulsifier is sodium dodecyl sulfate and dodecyl phenol polyoxyethylene ether according to the mass ratio of 1: 2, or a mixture thereof.

As a further scheme of the invention: the ratio of the prepolymer B to the aqueous potassium persulfate solution B in step A3 was 30 g: 100mL, wherein the mass fraction of the ammonia water is 10-15%.

As a further scheme of the invention: the preparation process of the modified heat-insulating nano powder dispersion liquid is as follows:

b1: adding acrylic acid and deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant pressure dropping funnel, and stirring at room temperature and a stirring speed of 500-;

b2: adding zinc acetate and gallium nitrate into the acrylic acid solution, continuously stirring for 20-50min, then dropwise adding the ammonium persulfate aqueous solution while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 10-30min after the dropwise adding is finished, and then continuously stirring and reacting for 20-30min under the condition of heating to 100 ℃ and 110 ℃ to obtain a nano powder precursor;

b3: placing the nano powder precursor in a vacuum drying box, drying for 2-3h at the temperature of 230-270 ℃, then taking out, cooling, grinding, then placing in a muffle furnace, and calcining for 3-4h at the temperature of 600-800 ℃ to obtain heat-insulating nano powder;

b4: adding the heat-insulating nano powder and an ethanol aqueous solution into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, and stirring for 30-60min under the condition that the stirring speed is 2000-3000r/min to obtain a heat-insulating nano powder dispersion liquid;

b5: adding a silane coupling agent KH-570 into an ethanol aqueous solution, uniformly stirring, then dropwise adding into the heat-insulating nano powder dispersion liquid while stirring at the temperature of 70-80 ℃ and the stirring speed of 800r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring and reacting for 2-3h after the dropwise adding is finished, then performing rotary evaporation until the ethanol is completely evaporated, and then performing ultrasonic dispersion for 10-20min under the condition that the ultrasonic frequency is 45-65kHz to obtain the modified heat-insulating nano powder dispersion liquid.

The reaction principle is as follows:

as a further scheme of the invention: the mass ratio of the acrylic acid to the deionized water in the step B1 is 7: 3; the mass ratio of the zinc acetate solution to the acrylic acid solution in the step B2 is 3: 20, the molar ratio of the zinc acetate to the gallium nitrate is 20-25: 1, the mass fraction of the ammonium persulfate aqueous solution is 2-5%, and the addition amount of the ammonium persulfate is 0.05-0.1 of the weight of acrylic acid.

As a further scheme of the invention: the ethanol aqueous solution in step B4 is absolute ethanol according to a ratio of 3: 1 is dissolved in deionized water to form a solution, and the dosage ratio of the heat-insulating nano powder to the ethanol water solution is 1 g: 20-50 mL; the dosage ratio of the silane coupling agent KH-570 to the ethanol aqueous solution in the step B5 is 1 g: 10-20mL, wherein the addition amount of the silane coupling agent KH-570 is 1.0-5.0% of the weight of the heat-insulating nano powder.

As a further scheme of the invention: a preparation method of high-light-transmission heat-insulation glass comprises the following steps:

the method comprises the following steps: weighing 100 parts of stain-resistant emulsion, 150 parts of modified heat-insulating nano powder dispersion liquid, 30-50 parts of film-forming assistant, 0.2-1 part of flatting agent, 0.2-1 part of defoaming agent and 10-30 parts of deionized water according to parts by weight;

step two: adding the stain-resistant emulsion into a mixer, sequentially adding deionized water, a film-forming aid and a flatting agent under the condition that the stirring rate is 400-600r/min, continuing to shear for 20-30min after the addition is finished, then adding the modified heat-insulating nano-powder dispersion liquid, continuing to shear for 1-2h under the condition that the stirring rate is 800-1100r/min, then adding a defoaming agent under the condition that the stirring rate is 100-300r/min, stirring for 10-20min, then standing for 2-3h, and filtering to obtain the heat-insulating coating;

step three: uniformly coating the heat-insulating coating on the surface of a cleaned glass substrate, naturally leveling, airing at room temperature under a dust-free condition, placing in an oven at 70 ℃ for drying for 1h after surface drying, and then placing at room temperature under the dust-free condition for 1-2h to obtain the high-light-transmission heat-insulating glass.

The invention has the beneficial effects that:

adding a stain-resistant emulsion into a mixer, sequentially adding deionized water, a film-forming aid and a leveling agent under the condition of stirring, continuing to shear after adding, then adding a modified heat-insulating nano powder dispersion liquid for continuing to shear, then adding a defoaming agent, stirring, standing and filtering to obtain a heat-insulating coating, uniformly coating the heat-insulating coating on the surface of a cleaned glass substrate, naturally leveling, airing at room temperature under a dust-free condition, placing in an oven for baking after surface drying, and then placing at room temperature under the dust-free condition to obtain the high-light-transmission heat-insulating glass; the high-light-transmission heat-insulation glass is characterized in that a heat-insulation coating is formed on a glass substrate and is formed by curing a heat-insulation coating, the heat-insulation coating has a self-cleaning stain-resistant effect while maintaining high light transmission through a stain-resistant emulsion, so that the high-light-transmission heat-insulation glass is difficult to adhere to stains and is easy to clean after adhering, the possibility that the light transmission of the glass is greatly reduced due to the stains is avoided, the heat-insulation coating can have an absorption heat-insulation effect through modifying heat-insulation nano powder dispersion liquid, and the glass is endowed with good heat-insulation performance;

methyl methacrylate, n-butyl acrylate, hydroxypropyl acrylate and dodecafluoroheptyl methacrylate are polymerized under the initiation action of potassium persulfate to form a high polymer, after dodecafluoroheptyl methacrylate is added, a large number of C-F bonds on the high polymer are the largest in chemical bond energy, and the high polymer can still keep high stability under the conditions of heating and illumination, so that the high-corrosion resistance and weather resistance are displayed, the fluorine atoms have the ultrahigh electronegativity, the repulsive force between adjacent fluorine atoms enables the C-C main chain to form a spiral structure, the fluorine atoms around the middle C-C main chain are closely adjacent to each other, the main carbon chain is completely surrounded to form a cylinder and high shielding, therefore, the coating can protect C-C bonds from being invaded by chemicals and ultraviolet rays, is suitable for being used as a material of a heat insulation coating, has good ultraviolet resistance, is suitable for the light heat insulation of glass, and directly causes the surface energy of the prepared heat insulation coating to be extremely low due to the existence of a large number of C-F bonds and low intermolecular force, so that the heat insulation coating is difficult to be soaked by water and organic matters, has good stain resistance, and avoids the reduction of the light permeability of the glass caused by stain pollution;

preparing the high-light-transmission heat-insulating glassThe preparation method comprises the steps of taking zinc acetate and gallium nitrate as raw materials, adding the raw materials into an acrylic acid solution to form acrylate, adding ammonium persulfate serving as an initiator in a polymerization reaction into the acrylic acid solution to promote the polymerization process to form a polyacrylate prepolymer with uniform ion distribution, acting zinc ions and gallium ions after polymerization and carboxyl on a polymer chain on the polymer chain through ionic bonds, and finally obtaining nanoscale gallium-doped zinc oxide powder with uniform components and structures in a pyrolysis process, namely the heat-insulating nano powder, wherein the zinc oxide is an important wide-bandgap II-VI oxide semiconductor material, belongs to an n-type semiconductor, has a direct band gap of 3.3eV, has good photoelectric properties, and Ga³⁺Ionic radius and Zn²⁺The ionic radii are very close, the reflection performance of a near infrared region of the nano heat-insulating powder can be obviously enhanced under proper preparation conditions and doping, and the nano heat-insulating powder has good visible light transmittance and infrared reflection effect, so that the transmittance of infrared light can be obviously reduced under the condition of ensuring high visible light transmittance, and the heat-insulating effect is achieved, and then the heat-insulating nano powder is modified by the silane coupling agent KH-570, the hydroxyl on the surface of the heat-insulating nano powder is eliminated, the aggregation of the heat-insulating nano powder is avoided, the dispersibility of the heat-insulating nano powder in the coating is enhanced, and the uniformity and the stability of the heat-insulating effect of the coating are ensured.

Detailed Description

The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1:

this example is a method of preparing a stain resistant emulsion comprising the steps of:

a1: adding 1/3 methyl methacrylate, 1/3 n-butyl acrylate and 1/3 hydroxypropyl acrylate into a beaker, stirring and dispersing for 30min at a stirring speed of 500r/min to obtain a prepolymer A, adding the rest of methyl methacrylate, n-butyl acrylate, hydroxypropyl acrylate and dodecafluoroheptyl methacrylate into another beaker, and stirring and dispersing for 30min at a stirring speed of 500r/min to obtain a prepolymer B; controlling the mol ratio of methyl methacrylate, n-butyl acrylate, hydroxypropyl acrylate and dodecafluoroheptyl methacrylate to be 0.1: 0.08: 0.04: 0.05;

a2: adding the prepolymer A and deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, dropwise adding a potassium persulfate aqueous solution A while stirring at a stirring speed of 300r/min, controlling the dropping speed to be 1 drop/s, heating to 50 ℃ after the dropwise adding is finished, adding an emulsifier, heating to 80 ℃ after the emulsifier is completely dissolved, and stirring for reacting for 20min to obtain an emulsion; controlling the dosage ratio of the prepolymer A, deionized water, a potassium persulfate aqueous solution A and an emulsifier to be 25 g: 100mL of: 10mL of: 1.2g, wherein the concentration of the potassium persulfate aqueous solution A is 6g/L, and the emulsifier is sodium dodecyl sulfate and dodecyl phenol polyoxyethylene ether according to the mass ratio of 1: 2;

a3: uniformly mixing the prepolymer B and a potassium persulfate aqueous solution B, then dropwise adding the mixture into the emulsion while stirring, controlling the dropping rate to be 1 s, stirring and reacting for 2-3h at the temperature of 80 ℃ after the dropping is finished, then cooling the reaction product to room temperature, and adding ammonia water to adjust the pH value to 7 to obtain a stain-resistant emulsion; controlling the using ratio of the prepolymer B to the potassium persulfate aqueous solution B to be 30 g: 100mL, and the mass fraction of the ammonia water is 10%.

Example 2:

this example is a method of preparing a stain resistant emulsion comprising the steps of:

a1: adding 1/3 methyl methacrylate, 1/3 n-butyl acrylate and 1/3 hydroxypropyl acrylate into a beaker, stirring and dispersing for 40min at a stirring speed of 800r/min to obtain a prepolymer A, adding the rest of methyl methacrylate, n-butyl acrylate, hydroxypropyl acrylate and dodecafluoroheptyl methacrylate into another beaker, and stirring and dispersing for 40min at a stirring speed of 800r/min to obtain a prepolymer B; controlling the mol ratio of methyl methacrylate, n-butyl acrylate, hydroxypropyl acrylate and dodecafluoroheptyl methacrylate to be 0.1: 0.08: 0.04: 0.05;

a2: adding the prepolymer A and deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant-pressure dropping funnel, dropwise adding a potassium persulfate aqueous solution A while stirring at a stirring speed of 500r/min, controlling the dropping speed to be 1 drop/s, heating to 55 ℃ after the dropwise adding is finished, adding an emulsifier, heating to 90 ℃ after the emulsifier is completely dissolved, stirring and reacting for 30min to obtain an emulsion; controlling the dosage ratio of the prepolymer A, deionized water, a potassium persulfate aqueous solution A and an emulsifier to be 25 g: 100mL of: 10mL of: 1.2g, wherein the concentration of the potassium persulfate aqueous solution A is 6g/L, and the emulsifier is sodium dodecyl sulfate and dodecyl phenol polyoxyethylene ether according to the mass ratio of 1: 2;

a3: uniformly mixing the prepolymer B and a potassium persulfate aqueous solution B, then dropwise adding the mixture into the emulsion while stirring, controlling the dropping rate to be 1 s, stirring and reacting for 3h at the temperature of 85 ℃ after the dropping is finished, then cooling the reaction product to room temperature, and adding ammonia water to adjust the pH value to 7 to obtain a stain-resistant emulsion; controlling the using ratio of the prepolymer B to the potassium persulfate aqueous solution B to be 30 g: 100mL, and the mass fraction of the ammonia water is 15%.

Example 3:

the embodiment is a preparation method of a modified nano heat insulation powder dispersion liquid, which comprises the following steps:

b1: adding acrylic acid and deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant pressure dropping funnel, and stirring at room temperature and a stirring speed of 500r/min until the acrylic acid and the deionized water are completely dissolved to obtain an acrylic acid solution; controlling the mass ratio of acrylic acid to deionized water to be 7: 3;

b2: adding zinc acetate and gallium nitrate into an acrylic acid solution, continuously stirring for 20min, then dropwise adding an ammonium persulfate aqueous solution while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 10min after the dropwise adding is finished, and then continuously stirring and reacting for 20min under the condition of heating to 100 ℃ to obtain a nano powder precursor; controlling the mass ratio of the zinc acetate to the acrylic acid solution to be 3: 20, the molar ratio of the zinc acetate to the gallium nitrate is 25: 1, the mass fraction of the ammonium persulfate aqueous solution is 2%, and the adding amount of the ammonium persulfate is 0.05 of the weight of acrylic acid;

b3: placing the nano powder precursor in a vacuum drying oven, drying for 2h at the temperature of 230 ℃, taking out, cooling, grinding, placing in a muffle furnace, and calcining for 3h at the temperature of 600 ℃ to obtain nano heat-insulating powder;

b4: adding the nanometer heat insulating powder and ethanol water solution into a three-neck flask provided with a stirrer, a thermometer and a constant pressure dropping funnel, and stirring for 30min under the condition that the stirring speed is 2000r/min to obtain nanometer heat insulating powder dispersion liquid; controlling the ethanol aqueous solution to be absolute ethanol according to the ratio of 3: 1 in deionized water, wherein the dosage ratio of the nanometer heat insulating powder to the ethanol aqueous solution is 1 g: 20 mL;

b5: adding a silane coupling agent KH-570 into an ethanol aqueous solution, uniformly stirring, then dropwise adding into the nano heat-insulating powder dispersion liquid while stirring at the temperature of 70 ℃ and the stirring speed of 500r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring and reacting for 2 hours after the dropwise adding is finished, then performing rotary evaporation until the ethanol is completely evaporated, and then performing ultrasonic dispersion for 10 minutes under the ultrasonic frequency of 45kHz to obtain a modified nano heat-insulating powder dispersion liquid; controlling the dosage ratio of the silane coupling agent KH-570 to the ethanol aqueous solution to be 1 g: 10mL, wherein the adding amount of the silane coupling agent KH-570 is 1.0 percent of the weight of the nano heat-insulating powder.

Example 4:

the embodiment is a preparation method of a modified nano heat insulation powder dispersion liquid, which comprises the following steps:

b1: adding acrylic acid and deionized water into a three-neck flask provided with a stirrer, a thermometer and a constant pressure dropping funnel, and stirring at room temperature and a stirring speed of 800r/min until the acrylic acid and the deionized water are completely dissolved to obtain an acrylic acid solution; controlling the mass ratio of acrylic acid to deionized water to be 7: 3;

b2: adding zinc acetate and gallium nitrate into an acrylic acid solution, continuously stirring for 50min, then dropwise adding an ammonium persulfate aqueous solution while stirring, controlling the dropwise adding speed to be 1 drop/s, continuously stirring for 30min after the dropwise adding is finished, and then continuously stirring and reacting for 30min under the condition of heating to 110 ℃ to obtain a nano powder precursor; controlling the mass ratio of the zinc acetate to the acrylic acid solution to be 3: 20, wherein the molar ratio of the zinc acetate to the gallium nitrate is 20: 1, the mass fraction of the ammonium persulfate aqueous solution is 5%, and the adding amount of the ammonium persulfate is 0.1 of the weight of acrylic acid;

b3: placing the nano powder precursor in a vacuum drying box, drying for 3h under the condition of temperature of 230-270 ℃, then taking out, cooling, grinding, then placing in a muffle furnace, and calcining for 4h under the condition of temperature of 800 ℃ to obtain nano heat-insulating powder;

b4: adding the nanometer heat insulating powder and ethanol water solution into a three-neck flask provided with a stirrer, a thermometer and a constant pressure dropping funnel, and stirring for 60min under the condition that the stirring speed is 3000r/min to obtain nanometer heat insulating powder dispersion liquid; controlling the ethanol aqueous solution to be absolute ethanol according to the ratio of 3: 1 in deionized water, wherein the dosage ratio of the nanometer heat insulating powder to the ethanol aqueous solution is 1 g: 50 mL;

b5: adding a silane coupling agent KH-570 into an ethanol aqueous solution, uniformly stirring, then dropwise adding into the nano heat-insulating powder dispersion liquid while stirring at the temperature of 80 ℃ and the stirring speed of 800r/min, controlling the dropwise adding speed to be 1 drop/s, continuously stirring and reacting for 3 hours after the dropwise adding is finished, then performing rotary evaporation until the ethanol is completely evaporated, and then performing ultrasonic dispersion for 20 minutes under the ultrasonic frequency of 65kHz to obtain the modified nano heat-insulating powder dispersion liquid; controlling the dosage ratio of the silane coupling agent KH-570 to the ethanol aqueous solution to be 1 g: 20mL, wherein the adding amount of the silane coupling agent KH-570 is 5.0 percent of the weight of the nano heat-insulating powder.

Example 5:

the embodiment is a preparation method of high-light-transmission heat-insulation glass, which comprises the following steps:

the method comprises the following steps: weighing 100 parts of the stain-resistant emulsion from example 1, 30 parts of the modified nano heat-insulating powder dispersion from example 3, 5 parts of a film-forming assistant, 0.2 part of a leveling agent, 0.2 part of a defoaming agent and 10 parts of deionized water in parts by weight;

step two: adding the stain-resistant emulsion into a mixer, sequentially adding deionized water, a film-forming aid and a flatting agent under the condition that the stirring speed is 400r/min, continuing to shear for 20min after the addition is finished, then adding the modified nano heat-insulating powder dispersion, continuing to shear for 1h under the condition that the stirring speed is 800r/min, then adding a defoaming agent under the condition that the stirring speed is 100r/min, stirring for 10min, then standing for 2h, and filtering to obtain a heat-insulating coating;

step three: uniformly coating the heat-insulating coating on the surface of a cleaned glass substrate, naturally leveling, airing at room temperature under a dust-free condition, placing in an oven at 70 ℃ for drying for 1h after surface drying, and then placing at room temperature under a dust-free condition for 1h to obtain the high-light-transmission heat-insulating glass.

Example 6:

the embodiment is a preparation method of high-light-transmission heat-insulation glass, which comprises the following steps:

the method comprises the following steps: weighing 150 parts of the stain-resistant emulsion from example 2, 50 parts of the modified nano heat-insulating powder dispersion from example 4, 10 parts of a film-forming assistant, 1 part of a leveling agent, 1 part of a defoaming agent and 30 parts of deionized water in parts by weight;

step two: adding the stain-resistant emulsion into a mixer, sequentially adding deionized water, a film-forming aid and a flatting agent under the condition that the stirring speed is 600r/min, continuing to shear for 30min after the addition is finished, then adding the modified nano heat-insulating powder dispersion, continuing to shear for 2h under the condition that the stirring speed is 1100r/min, then adding a defoaming agent under the condition that the stirring speed is 300r/min, stirring for 20min, standing for 3h, and filtering to obtain a heat-insulating coating;

step three: uniformly coating the heat-insulating coating on the surface of a cleaned glass substrate, naturally leveling, airing at room temperature under a dust-free condition, placing in an oven at 70 ℃ for drying for 1h after surface drying, and then placing at room temperature under a dust-free condition for 2h to obtain the high-light-transmission heat-insulating glass.

Comparative example 1:

this comparative example differs from example 6 in that a styrene-acrylic emulsion was used instead of the stain-resistant emulsion.

Comparative example 2:

this comparative example is different from example 6 in that ATO nano-ions are used instead of the modified nano-thermal insulation powder dispersion.

The performances of examples 5 to 6 and comparative examples 1 to 2 were examined. Contact angle: the contact angle of the thermal barrier coating with water was measured on contact angle measuring instrument JC2000C 1. Each measurement was completed within 10 seconds after the droplet was in contact with the surface, and the results were averaged over 10 times. Heat insulation performance: reference is made to the 1976 standard of the American military Standard MIL-E-46136 (A). The maximum temperature difference of the high-light-transmission heat-insulating glass compared with the blank glass is tested. Transmittance: and measuring the optical transmittance of the coated glass at 300-.

The results are shown in the following table:

sample (I)	Average transmittance in the visible region/%)	Maximum temperature difference/. degree.C	Contact Angle/°
				Example 5	79.1	14	141
Example 6	83.6	17	145
				Comparative example 1	51.8	11	105
Comparative example 2	62.9	8	133

According to the comparison between the example and the comparative example 1, the light transmittance and the contact angle of the stain-resistant emulsion to the coating are obviously improved, so that the glass has self-cleaning stain-resistant performance while keeping high light transmittance, the possibility of light transmittance reduction caused by stain pollution is reduced, and the heat resistance of the modified nano heat-insulating powder is good through the comparison between the example and the comparative example 2.

In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.