Preparation method of full-shield infrared and ultraviolet transparent paint with self-cleaning function

Abstract

The application relates to a preparation method of a full-shielding infrared and ultraviolet transparent paint with a self-cleaning function, which belongs to the field of building environment-friendly materials. The method comprises the following steps: one, sequentially adding water-based fluorosilicon emulsion, deionized water, hydrophobic WO3-coated nanometer cesium tungsten bronze composite material and nanometer indium tin oxide-titanium dioxide compound into a dispersing tank for dispersion; two, grinding and then transferring into the dispersing tank for dispersion; three, adding an additive into the dispersing tank for continuous dispersion, so as to obtain the full-shielding infrared and ultraviolet transparent paint with the self-cleaning function. The transparent coating formed after the full-shielding infrared and ultraviolet transparent paint with the self-cleaning function prepared by the application is coated on glass, can shield more than 99% of infrared light and ultraviolet light, and can transmit more than 70% of visible light through the glass, so that the heat insulation and cooling effect of the glass is greatly improved without affecting the transparency of the glass, and the paint has good self-cleaning and stain resistance.

Description

Technical Field

[0001] This invention pertains to environmentally friendly building materials, specifically relating to a method for preparing a fully shielded transparent coating with self-cleaning properties that blocks infrared and ultraviolet rays. Background Technology

[0002] In the construction sector, energy consumption is a particularly prominent issue. Statistics show that building energy consumption accounts for 30% of total social energy consumption, and air conditioning energy consumption accounts for 65% of building energy consumption, as well as 10% of global greenhouse gas emissions, with this trend gradually increasing. Existing ordinary building windows cannot block infrared light energy, a significant factor contributing to excessive air conditioning energy consumption in buildings during summer. While LOW-E glass on the market cannot be widely used due to its low light transmittance and price, a transparent glass coating with good thermal insulation performance, simple manufacturing process, low cost, and scalable application has been developed to meet the thermal insulation needs of building glass.

[0003] Solar radiation is the main source of energy consumption for air conditioning systems, with heat entering the building through translucent glass accounting for 70% of air conditioning energy consumption. Visible light (380-780nm band) accounts for 45% of the total solar radiation energy, ultraviolet light (300-380nm) accounts for 5%, and near-infrared light (780-2500nm band) accounts for 50%. Therefore, blocking the transmission of infrared and ultraviolet light while ensuring that visible light can pass through the glass can achieve indoor heat insulation and cooling.

[0004] Existing infrared shielding materials are mostly one or a combination of nanomaterials such as indium tin oxide or antimony tin oxide. However, the films prepared using these materials have low transparency, and their infrared and ultraviolet blocking rates are less than 80%, often failing to meet the thermal insulation and cooling requirements of modern glass. The low-E glass commonly used in modern building curtain walls has low visible light transmittance, severely impacting indoor lighting. Therefore, there is an urgent need to find a glass film with high transparency and excellent cooling performance to replace traditional low-E glass. Summary of the Invention

[0005] To address the aforementioned technical problems, this invention provides a method for preparing a fully shielded infrared and ultraviolet transparent coating with self-cleaning function.

[0006] The transparent coating formed by applying a self-cleaning, fully shielding infrared and ultraviolet transparent coating to glass prepared using this invention can block more than 99% of infrared and ultraviolet light, while allowing more than 70% of visible light to pass through the glass. This greatly improves the heat insulation and cooling effect of the glass without affecting its transparency. Furthermore, the coating has good self-cleaning and stain resistance properties.

[0007] A method for preparing a self-cleaning, fully shielded, transparent coating against infrared and ultraviolet rays is specifically carried out according to the following steps:

[0008] 1. Water-based fluorosilicone emulsion, deionized water, hydrophobic WO3-coated nano-cesium tungsten bronze composite material and nano-indium tin oxide-titanium dioxide composite material are sequentially added to a dispersion tank and dispersed at a certain speed for a period of time to obtain a dispersion.

[0009] 2. Place the above dispersion in a high-speed vibrating mill and grind it at a certain speed for a period of time. Then, export the dispersion into a dispersion tank and continue to disperse it for a period of time.

[0010] 3. Add additives to the dispersion tank and continue to disperse for a period of time to obtain a transparent coating that fully shields infrared and ultraviolet rays with self-cleaning function;

[0011] The preparation method of the hydrophobic WO3-coated nano-cesium tungsten bronze composite material is specifically carried out according to the following steps:

[0012] (1) Preparation of nano-cesium tungsten bronze:

[0013] ① Mix tungsten hexachloride, cesium chloride, citric acid and polyethylene glycol evenly, heat and stir for a period of time to obtain a mixture;

[0014] ② Transfer the mixture to a hydrothermal reactor and react it hydrothermally at 220℃~240℃ for 24h~26h to obtain the reaction product; centrifuge the reaction product and dry the centrifuged material to obtain nano-cesium tungsten bronze particles;

[0015] (2) Dissolve Na2WO4·2H2O in an ethanol solution, and then acidify the solution to a pH of 1.0-3.0 using sulfuric acid with a mass fraction of 95%-98% to obtain the reaction solution;

[0016] (3) Add nano-cesium tungsten bronze particles to the reaction solution, then heat to 120℃~140℃, stir and react at 120℃~140℃ for a period of time to obtain WO3-coated nano-cesium tungsten bronze composite material.

[0017] (4) First, the WO3-coated nano-cesium tungsten bronze composite material is added to an octadecyltrichlorosilane anhydrous ethanol solution with a mass fraction of 0.5% to 1% for 2 to 4 hours. Then, it is washed by centrifugation with anhydrous ethanol 2 to 4 times, and then dried at 50℃ to 70℃ for 4 to 6 hours to obtain a hydrophobic WO3-coated nano-cesium tungsten bronze composite material.

[0018] The preparation method of the aforementioned nano-indium tin oxide-titanium dioxide composite is specifically carried out according to the following steps:

[0019] I. Add nano-indium tin oxide to anhydrous ethanol, then disperse it ultrasonically under ice bath conditions, stir it, and finally add deionized water, tetrabutyl titanate, polyvinylpyrrolidone, citric acid, oleic acid and stearic acid under magnetic stirring to obtain a mixed solution.

[0020] II. The mixed solution was ball-milled for a period of time, then washed, freeze-dried, and ground to obtain nano-indium tin oxide-titanium dioxide composite.

[0021] The principles and advantages of this invention:

[0022] I. Cesium tungsten bronze (CsxWO3), as a non-stoichiometric functional compound with a special oxygen octahedral structure, has stronger near-infrared blocking performance than indium tin oxide or antimony tin oxide. Nano-WO3 has a good shielding effect on electromagnetic radiation X-rays with wavelengths between 200nm and 400nm that are harmful to the human body, which are between ultraviolet and gamma rays. At the same time, tungsten oxide has a certain shielding effect on both long-wave and short-wave near-infrared rays, and has high visible light transmittance. This invention uses WO3 to coat cesium tungsten bronze to shield the harmful wavelengths, enhance the shielding effect of infrared and ultraviolet rays, and endow the coating with a "light response" intelligent adjustment function. It uses octadecyltrichlorosilane anhydrous ethanol solution to modify WO3-coated cesium tungsten bronze, giving it self-cleaning properties.

[0023] II. The present invention prepares a nano-indium tin oxide-titanium dioxide composite, which can shield infrared and ultraviolet rays, and also has high transmittance and self-cleaning and decontamination ability.

[0024] Third, the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared by this invention can be applied to the glass surface by spraying, rolling, or brushing. Existing windows can be coated without replacing the glass, and the coating can be repaired later if it is damaged.

[0025] IV. The coating obtained by using the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared by the present invention has high visible light transmittance. Compared with other glass film materials, it can block more than 99% of infrared and ultraviolet light, and has excellent heat insulation and cooling effect.

[0026] V. The coating obtained by using the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared by the present invention has excellent self-cleaning function and is expected to be widely used as a new material in the field of building and automotive glass insulation. Attached Figure Description

[0027] Figure 1 The water contact angle test diagram is shown for a tinplate sample coated with a self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 1 of the present invention.

[0028] Figure 2 The water contact angle test diagram is shown for a tinplate sample coated with a self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 2 of the present invention.

[0029] Figure 3 The water contact angle test diagram is shown for the tinplate sample coated with the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 3 of the present invention. Detailed Implementation

[0030] Specific Implementation Method 1: This implementation method provides a method for preparing a fully shielded transparent coating with self-cleaning function that blocks infrared and ultraviolet rays, specifically completed according to the following steps:

[0031] 1. Water-based fluorosilicone emulsion, deionized water, hydrophobic WO3-coated nano-cesium tungsten bronze composite material and nano-indium tin oxide-titanium dioxide composite material are sequentially added to a dispersion tank and dispersed at a certain speed for a period of time to obtain a dispersion.

[0032] 2. Place the above dispersion in a high-speed vibrating mill and grind it at a certain speed for a period of time. Then, export the dispersion into a dispersion tank and continue to disperse it for a period of time.

[0033] 3. Add additives to the dispersion tank and continue to disperse for a period of time to obtain a transparent coating that fully shields infrared and ultraviolet rays with self-cleaning function;

[0034] The preparation method of the hydrophobic WO3-coated nano-cesium tungsten bronze composite material is specifically carried out according to the following steps:

[0035] (1) Preparation of nano-cesium tungsten bronze:

[0036] ① Mix tungsten hexachloride, cesium chloride, citric acid and polyethylene glycol evenly, heat and stir for a period of time to obtain a mixture;

[0037] ② Transfer the mixture to a hydrothermal reactor and react it hydrothermally at 220℃~240℃ for 24h~26h to obtain the reaction product; centrifuge the reaction product and dry the centrifuged material to obtain nano-cesium tungsten bronze particles;

[0038] (2) Dissolve Na2WO4·2H2O in an ethanol solution, and then acidify the solution to a pH of 1.0-3.0 using sulfuric acid with a mass fraction of 95%-98% to obtain the reaction solution;

[0039] (3) Add nano-cesium tungsten bronze particles to the reaction solution, then heat to 120℃~140℃, stir and react at 120℃~140℃ for a period of time to obtain WO3-coated nano-cesium tungsten bronze composite material.

[0040] (4) First, the WO3-coated nano-cesium tungsten bronze composite material is added to an octadecyltrichlorosilane anhydrous ethanol solution with a mass fraction of 0.5% to 1% for 2 to 4 hours. Then, it is washed by centrifugation with anhydrous ethanol 2 to 4 times, and then dried at 50℃ to 70℃ for 4 to 6 hours to obtain a hydrophobic WO3-coated nano-cesium tungsten bronze composite material.

[0041] The preparation method of the aforementioned nano-indium tin oxide-titanium dioxide composite is specifically carried out according to the following steps:

[0042] I. Add nano-indium tin oxide to anhydrous ethanol, then disperse it ultrasonically under ice bath conditions, stir it, and finally add deionized water, tetrabutyl titanate, polyvinylpyrrolidone, citric acid, oleic acid and stearic acid under magnetic stirring to obtain a mixed solution.

[0043] II. The mixed solution was ball-milled for a period of time, then washed, freeze-dried, and ground to obtain nano-indium tin oxide-titanium dioxide composite.

[0044] Specific Implementation Method Two: This implementation method differs from Specific Implementation Method One in that: in step one, the aqueous fluorosilicone emulsion, deionized water, hydrophobic WO3-coated nano-cesium tungsten bronze composite material, and nano-indium tin oxide-titanium dioxide composite are sequentially added to a dispersion tank and dispersed uniformly at a speed of 1000 r / min for 30 min to 60 min to obtain a dispersion. Other steps are the same as in Specific Implementation Method One.

[0045] Specific Implementation Method Three: This implementation method differs from Specific Implementation Method One or Two in that: In step two, the above dispersion is placed in a high-speed vibrating mill and ground at 1000-3000 r / min for 30-60 minutes, then the dispersion is transferred to a dispersion tank and dispersed again at 1000 r / min for 30-60 minutes; in step three, the dispersion time is 20-40 minutes. Other steps are the same as in Specific Implementation Method One or Two.

[0046] Specific Implementation Method Four: This implementation method differs from Specific Implementation Methods One to Three in that: the mass fraction of the aqueous fluorosilicone emulsion in the dispersion in step one is not less than 30%; the mass ratio of the aqueous fluorosilicone emulsion, the hydrophobic WO3-coated nano-cesium tungsten bronze composite material, and the nano-indium tin oxide-titanium dioxide composite material in step one is 1:(0.5-1):(0.1-3). Other steps are the same as in Specific Implementation Methods One to Three.

[0047] Specific Implementation Method Five: This implementation method differs from Specific Implementation Methods One to Four in that the fineness of the dispersion after grinding in step two does not exceed 100 nm. The other steps are the same as in Specific Implementation Methods One to Four.

[0048] Specific Implementation Method Six: This implementation method differs from Specific Implementation Methods One to Five in that: the additives mentioned in step three include dispersants, defoamers, wetting agents, leveling agents, and thickeners. The dispersant is one or a combination of several of the following: a high molecular weight block copolymer solution containing pigment affinity groups, an aqueous solution containing polymers with high pigment affinity groups, and a surfactant. The defoamer is one or a combination of several of the following: a polyether siloxane copolymer and a mineral oil defoamer. The wetting agent is one or a combination of several of the following: a polyether siloxane copolymer, a polyether-modified siloxane, and an organosilicon twin-structure surfactant. The leveling agent is one or a combination of several of the following: a polyacrylate leveling agent, a polyurethane leveling agent, and an organosilicon leveling agent. The thickener is one or a combination of several of the following: a polyurethane or a polyacrylate thickener. The other steps are the same as in Specific Implementation Methods One to Five.

[0049] Specific Implementation Method Seven: This implementation method differs from Specific Implementation Methods One to Six in that the mass ratio of the dispersant, defoamer, wetting agent, leveling agent, and thickener is 1:(0.1-0.3):(0.1-0.2):(0.1-0.2):(0.1-0.2). The other steps are the same as in Specific Implementation Methods One to Six.

[0050] Specific Implementation Method Eight: This implementation method differs from Specific Implementation Methods One to Seven in that the mass fraction of the additives in the self-cleaning, fully shielded infrared and ultraviolet transparent coating described in step three does not exceed 5%. The other steps are the same as in Specific Implementation Methods One to Seven.

[0051] Specific Implementation Method Nine: The difference between this implementation method and Specific Implementation Methods One to Eight is as follows: the molar ratio of tungsten hexachloride to cesium chloride in step (1)① is 3:(0.5~1); the mass ratio of the total mass of tungsten hexachloride and cesium chloride to citric acid in step (1)① is (10~20):(20~50); the mass ratio of the total mass of tungsten hexachloride and cesium chloride to polyethylene glycol in step (1)① is (10~20):(10~30); the heating and stirring temperature in step (1)① is 60℃~90℃, and the heating and stirring time is 1h~2h; the mass fraction of the ethanol solution in step (2) is 10%~40%; the mass ratio of the total mass of tungsten hexachloride and cesium chloride to polyethylene glycol in step (1)① is 10%~40%; the mass ratio of the total mass of tungsten hexachloride and cesium chloride to polyethylene glycol in step (1)① is 10%~40%; the mass ratio of the total mass of tungsten hexachloride and cesium chloride to polyethylene glycol in step (1)① is 10%~9 ...90%; the mass ratio of the total mass of tungsten hexachloride and cesium chloride to polyethylene glycol in step (1)① is 10%~90%; the mass ratio of the total mass of The mass ratio of Na2WO4·2H2O to the volume ratio of the ethanol solution is (0.5g~1g):50mL; the stirring reaction time in step (3) is 20h~50h; the stirring speed in step (3) is 500r / min~1000r / min; the mass ratio of the nano-cesium tungsten bronze particles to the volume ratio of the reaction solution in step (3) is (0.05g~0.1g):(1mL~3mL); the mass ratio of the WO3-coated nano-cesium tungsten bronze composite material to the volume ratio of 0.5%~1% octadecyltrichlorosilane anhydrous ethanol solution in step (4) is (1g~3g):(5mL~10mL). Other steps are the same as in specific embodiments one to eight.

[0052] Specific Implementation Method Ten: This implementation method differs from Specific Implementation Methods One to Nine in the following ways: the ultrasonic dispersion time in step I is 30-60 minutes; the stirring time is 10-20 minutes; the mass-to-volume ratio of nano-indium tin oxide, deionized water, and anhydrous ethanol in step I is (0.5g-1g):(1g-2g):(100mL-200mL); the tetrabutyl titanate, polyvinylpyrrolidone, citric acid, oleic acid, and stearic acid in step I are... The mass-to-volume ratio of anhydrous ethanol is (15g-20g):(15g-20g):(1g-2g):(1.5g-2g):(10g-25g):(100mL-200mL); the ball milling time in step II is 0.5h-1h; the cleaning in step II involves alternating between anhydrous ethanol and deionized water, cleaning 3-5 times each; the freeze-drying temperature in step II is -45℃ to -55℃, and the freeze-drying time is 20h-24h. Other steps are the same as in specific embodiments one through nine.

[0053] The beneficial effects of the present invention are verified using the following embodiments:

[0054] Example 1: A method for preparing a self-cleaning, fully shielded transparent coating against infrared and ultraviolet rays, specifically comprising the following steps:

[0055] 1. 50g of aqueous fluorosilicone emulsion with a solid content of 45%, 13g of deionized water, 30g of hydrophobic WO3-coated nano-cesium tungsten bronze composite material and 5g of nano-indium tin oxide-titanium dioxide composite were sequentially added into a dispersion tank and dispersed uniformly at a speed of 1000r / min for 30min to obtain a dispersion.

[0056] 2. Place the above dispersion in a high-speed vibrating mill and disperse it uniformly at a speed of 3000 r / min for 60 min. Then export the dispersion to a dispersion tank and disperse it at a speed of 1000 r / min for 30 min.

[0057] 3. Add 1.2g of polyurethane dispersant, 0.12g of silicone oil defoamer, 0.24g of polyether siloxane activator, 0.24g of polyacrylate leveling agent and 0.2g of alkali-swelling thickener to the dispersion tank, and disperse evenly at a speed of 3000r / min for 60min to obtain a fully shielded infrared and ultraviolet transparent coating with self-cleaning function.

[0058] The aqueous fluorosilicone emulsion is HydroGuard 2000 fluorosilicone emulsion, purchased from Ao Ke New Materials Technology (Shanghai) Co., Ltd.

[0059] The polyurethane dispersant mentioned is DIGIC 760W dispersant, purchased from Shanghai Deyude Trading Co., Ltd.

[0060] The aforementioned silicone oil defoamer is MSD-916 polyether modified silicone oil, purchased from Qingdao Meiside Organosilicon Co., Ltd.

[0061] The polyether siloxane activator mentioned above is Tegopren 5840, which was purchased from Jining Tangyi Chemical Co., Ltd.

[0062] The polyacrylate leveling agent mentioned is PERENOL F45 leveling agent, purchased from Shenzhen Longdi Chemical Co., Ltd.

[0063] The alkali-swellable thickener mentioned is ASE-60, purchased from Qingdao Enze Chemical Co., Ltd.

[0064] The preparation method of the hydrophobic WO3-coated nano-cesium tungsten bronze composite material is specifically carried out according to the following steps:

[0065] (1) Preparation of nano-cesium tungsten bronze:

[0066] ① Mix tungsten hexachloride, cesium chloride, citric acid and polyethylene glycol evenly, and heat and stir at 80°C for 1.5 hours to obtain a mixture;

[0067] The molar ratio of tungsten hexachloride to cesium chloride mentioned in step (1)① is 3:1;

[0068] The total mass ratio of tungsten hexachloride and cesium chloride mentioned in step (1)① to citric acid is 15:40;

[0069] The total mass ratio of tungsten hexachloride and cesium chloride to polyethylene glycol in step (1)① is 15:20;

[0070] ② The mixture is transferred to a hydrothermal reactor and then hydrothermally reacted at 230°C for 24 hours to obtain the reaction product; the reaction product is centrifuged and the centrifuged material is dried to obtain nano-cesium tungsten bronze particles;

[0071] (2) Dissolve Na2WO4·2H2O in an ethanol solution, and then acidify the solution to pH 1.0 using 98% sulfuric acid to obtain the reaction solution;

[0072] The ethanol solution mentioned in step (2) has a mass fraction of 15%;

[0073] The mass ratio of Na2WO4·2H2O to the volume ratio of the ethanol solution in step (2) is 1g:50mL;

[0074] (3) Add nano-cesium tungsten bronze particles to the reaction solution, then heat to 130°C, and stir the reaction at 130°C for 40 hours to obtain WO3-coated nano-cesium tungsten bronze composite material.

[0075] The stirring speed mentioned in step (3) is 500 r / min;

[0076] The mass ratio of the nano-cesium tungsten bronze particles to the volume ratio of the reaction solution in step (3) is 0.1 g: 3 mL;

[0077] (4) First, the WO3-coated nano-cesium tungsten bronze composite material was added to an octadecyltrichlorosilane anhydrous ethanol solution with a mass fraction of 0.6% for 3 hours. Then, it was washed three times by centrifugation with anhydrous ethanol and dried at 60°C for 5 hours to obtain a hydrophobic WO3-coated nano-cesium tungsten bronze composite material.

[0078] The mass ratio of the WO3-coated nano-cesium tungsten bronze composite material to the 0.6% octadecyltrichlorosilane anhydrous ethanol solution in step (4) is 1 g: 5 mL.

[0079] The preparation method of the aforementioned nano-indium tin oxide-titanium dioxide composite is specifically carried out according to the following steps:

[0080] I. Add nano-indium tin oxide to anhydrous ethanol, then ultrasonically disperse for 30 min under ice bath conditions, then stir for 20 min, and finally add deionized water, tetrabutyl titanate, polyvinylpyrrolidone, citric acid, oleic acid and stearic acid under magnetic stirring to obtain a mixed solution.

[0081] The mass-to-volume ratio of nano-indium tin oxide, deionized water, and anhydrous ethanol mentioned in step I is 0.5g:1.5g:150mL;

[0082] The mass ratio of tetrabutyl titanate, polyvinylpyrrolidone, citric acid, oleic acid, stearic acid and the volume ratio of anhydrous ethanol in step I are 15g:20g:1.5g:1.5g:20g:150mL.

[0083] II. The mixed solution was ball-milled for 1 hour, then washed, freeze-dried, and ground to obtain nano-indium tin oxide-titanium dioxide composite.

[0084] The cleaning described in step II involves alternating between anhydrous ethanol and deionized water, and cleaning three times for each.

[0085] The freeze-drying temperature in step II is -55℃, and the freeze-drying time is 24 hours.

[0086] The self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 1 was filtered through a 300-mesh ultrafine filter. Then, the coating was uniformly coated onto a tinplate sample and a 5mm thick float glass surface using a 20μm coating blade. After the coating was naturally dried for 120 minutes, the performance parameters were tested, as shown in Table 1. The glass obtained using the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 1 of this invention is cooling glass.

[0087] Table 1 Optical performance parameters of commercially available float glass and cooling glass prepared in Example 1

[0088]

[0089] Figure 1 The water contact angle test diagram is shown for a tinplate sample coated with a self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 1 of the present invention.

[0090] from Figure 1 It can be seen that the water contact angle of the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 1 of the present invention when applied to the tinplate sample is 145°.

[0091] Example 2: The difference between this example and Example 1 is that in step one, 50g of aqueous fluorosilicone emulsion with a solid content of 45%, 13g of deionized water, 25g of hydrophobic WO3-coated nano-cesium tungsten bronze composite material, and 10g of nano-indium tin oxide-titanium dioxide composite were sequentially added to a dispersion tank and dispersed uniformly at a speed of 1000 r / min for 30 min to obtain a dispersion. Other steps and parameters are the same as in Example 1.

[0092] The self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 2 was filtered through a 300-mesh ultrafine filter. Then, the coating was uniformly coated onto a tinplate sample and a 5mm thick float glass surface using a 20μm scraper. After the coating was allowed to dry naturally for 120 minutes, the performance parameters were tested, as shown in Table 2. The glass obtained using the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 2 of this invention is a cooling glass.

[0093] Table 2 Optical performance parameters of commercially available float glass and cooling glass prepared in Example 2

[0094]

[0095] Figure 2 The water contact angle test diagram is shown for a tinplate sample coated with a self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 2 of the present invention.

[0096] from Figure 2 It can be seen that the water contact angle of the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 2 of the present invention when coated on the tinplate sample is 147°.

[0097] Example 3: The difference between this example and Example 1 is that in step one, 45g of aqueous fluorosilicone emulsion with a solid content of 45%, 13g of deionized water, 35g of hydrophobic WO3-coated nano-cesium tungsten bronze composite material, and 5g of nano-indium tin oxide-titanium dioxide composite were sequentially added to a dispersion tank and dispersed uniformly at a speed of 1000 r / min for 30 min to obtain a dispersion. Other steps and parameters are the same as in Example 1.

[0098] The self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 3 was filtered through a 300-mesh ultrafine filter. Then, the coating was uniformly coated onto a tinplate sample and a 5mm thick float glass surface using a 20μm scraper. After the coating was naturally dried for 120 minutes, the performance parameters were tested, as shown in Table 3. The glass obtained using the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 3 of this invention is cooling glass.

[0099] Table 3 Optical performance parameters of commercially available float glass and cooling glass prepared in Example 3

[0100]

[0101]

[0102] Figure 3 The water contact angle test diagram is shown for the tinplate sample coated with the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 3 of the present invention.

[0103] from Figure 3 It can be seen that the water contact angle of the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Example 3 of the present invention when coated on the tinplate sample is 141°.

[0104] Comparative Example 1: The specific method for preparing the coating in this embodiment is as follows:

[0105] 1. Add 50g of aqueous fluorosilicone emulsion with a solid content of 45%, 13g of deionized water, 30g of nano cesium tungsten bronze and 5g of nano indium tin oxide into a dispersion tank in sequence, and disperse at a speed of 1000r / min for 30min to obtain a dispersion.

[0106] 2. Place the above dispersion in a high-speed vibrating mill and disperse it uniformly at a speed of 3000 r / min for 60 min. Then export the dispersion to a dispersion tank and disperse it at a speed of 1000 r / min for 30 min.

[0107] 3. Add 1.2g of polyurethane dispersant, 0.12g of silicone oil defoamer, 0.24g of polyether siloxane activator, 0.24g of polyacrylate leveling agent and 0.2g of alkali-swelling thickener to the dispersion tank, and disperse evenly at a speed of 3000r / min for 60min to obtain a fully shielded infrared and ultraviolet transparent coating with self-cleaning function.

[0108] The aqueous fluorosilicone emulsion is HydroGuard 2000 fluorosilicone emulsion, purchased from Ao Ke New Materials Technology (Shanghai) Co., Ltd.

[0109] The polyurethane dispersant mentioned is DIGIC 760W dispersant, purchased from Shanghai Deyude Trading Co., Ltd.

[0110] The aforementioned silicone oil defoamer is MSD-916 polyether modified silicone oil, purchased from Qingdao Meiside Organosilicon Co., Ltd.

[0111] The polyether siloxane activator mentioned above is Tegopren 5840, which was purchased from Jining Tangyi Chemical Co., Ltd.

[0112] The polyacrylate leveling agent mentioned is PERENOL F45 leveling agent, purchased from Shenzhen Longdi Chemical Co., Ltd.

[0113] The alkali-swellable thickener mentioned is ASE-60, which was purchased from Qingdao Enze Chemical Co., Ltd.

[0114] The self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Comparative Example 1 was filtered through a 300-mesh ultrafine filter. Then, the coating was uniformly coated onto a tinplate sample and a 5mm thick float glass surface using a 20μm scraper. After the coating was allowed to dry naturally for 120 minutes, the performance parameters were tested, as shown in Table 4. The glass obtained using the self-cleaning, fully shielded infrared and ultraviolet transparent coating prepared in Comparative Example 1 of this invention is a cooling glass.

[0115] Table 4 Optical performance parameters of commercially available float glass and cooling glass prepared in Control Example 1

[0116]

Claims

1. A method for preparing a fully shielded infrared and ultraviolet transparent coating with self-cleaning function, characterized in that... The preparation method is specifically carried out according to the following steps:

1. Water-based fluorosilicone emulsion, deionized water, hydrophobic WO3-coated nano-cesium tungsten bronze composite material and nano-indium tin oxide-titanium dioxide composite material are sequentially added to a dispersion tank and dispersed at a certain speed for a period of time to obtain a dispersion.

2. Place the above dispersion in a high-speed vibrating mill and grind it at a certain speed for a period of time. Then, export the dispersion into a dispersion tank and continue to disperse it for a period of time.

3. Add additives to the dispersion tank and continue to disperse for a period of time to obtain a transparent coating that fully shields infrared and ultraviolet rays with self-cleaning function; The preparation method of the hydrophobic WO3-coated nano-cesium tungsten bronze composite material is specifically carried out according to the following steps: (1) Preparation of nano-cesium tungsten bronze: ① Mix tungsten hexachloride, cesium chloride, citric acid and polyethylene glycol evenly, heat and stir for a period of time to obtain a mixture; ② Transfer the mixture to a hydrothermal reactor and react it hydrothermally at 220℃~240℃ for 24h~26h to obtain the reaction product; centrifuge the reaction product and dry the centrifuged material to obtain nano-cesium tungsten bronze particles; (2) Dissolve Na2WO4·2H2O in an ethanol solution, and then acidify the solution to a pH value of 1.0~3.0 using sulfuric acid with a mass fraction of 95%~98% to obtain the reaction solution; (3) Add nano-cesium tungsten bronze particles to the reaction solution, then heat to 120℃~140℃, stir and react at 120℃~140℃ for a period of time to obtain WO3-coated nano-cesium tungsten bronze composite material. (4) First, the WO3-coated nano-cesium tungsten bronze composite material is added to an octadecyltrichlorosilane anhydrous ethanol solution with a mass fraction of 0.5%~1% for 2h~4h, then centrifuged and washed 2~4 times with anhydrous ethanol, and then dried at 50℃~70℃ for 4h~6h to obtain hydrophobic WO3-coated nano-cesium tungsten bronze composite material. The preparation method of the aforementioned nano-indium tin oxide-titanium dioxide composite is specifically carried out according to the following steps: I. Add nano-indium tin oxide to anhydrous ethanol, then disperse it ultrasonically under ice bath conditions, stir it, and finally add deionized water, tetrabutyl titanate, polyvinylpyrrolidone, citric acid, oleic acid and stearic acid under magnetic stirring to obtain a mixed solution. II. The mixed solution was ball-milled for a period of time, then washed, freeze-dried, and ground to obtain nano-indium tin oxide-titanium dioxide composite.

2. The method for preparing a self-cleaning, fully shielded infrared and ultraviolet transparent coating according to claim 1, characterized in that... In step one, the aqueous fluorosilicone emulsion, deionized water, hydrophobic WO3-coated nano-cesium tungsten bronze composite material and nano-indium tin oxide-titanium dioxide composite material are sequentially added to a dispersion tank and dispersed uniformly at a speed of 1000 r / min for 30 min to 60 min to obtain a dispersion.

3. The method for preparing a self-cleaning, fully shielded infrared and ultraviolet transparent coating according to claim 1, characterized in that... In step two, the above dispersion is placed in a high-speed vibrating mill and ground at 1000~3000 r / min for 30 min~60 min. Then, the dispersion is exported and placed in a dispersion tank and dispersed at 1000 r / min for another 30 min~60 min. In step three, the dispersion is continued for 20 min~40 min.

4. The method for preparing a self-cleaning, fully shielded infrared and ultraviolet transparent coating according to claim 1, characterized in that... The mass fraction of the aqueous fluorosilicone emulsion in the dispersion in step one is not less than 30%; the mass ratio of the aqueous fluorosilicone emulsion, the hydrophobic WO3-coated nano-cesium tungsten bronze composite material, and the nano-indium tin oxide-titanium dioxide composite material in step one is 1:(0.5~1):(0.1~3).

5. The method for preparing a self-cleaning, fully shielded infrared and ultraviolet transparent coating according to claim 1, characterized in that... In step two, the dispersion is ground to a fineness of no more than 100 nm.

6. The method for preparing a self-cleaning, fully shielded infrared and ultraviolet transparent coating according to claim 1, characterized in that... The additives mentioned in step three include dispersants, defoamers, wetting agents, leveling agents, and thickeners. The dispersant is one or a combination of several of the following: a high molecular weight block copolymer solution containing pigment affinity groups, an aqueous solution containing polymers with high pigment affinity groups, and a surfactant. The defoamer is one or a combination of several of the following: a polyether siloxane copolymer and a mineral oil defoamer. The wetting agent is one or a combination of several of the following: a polyether siloxane copolymer, a polyether-modified siloxane, and an organosilicon twin-structure surfactant. The leveling agent is one or a combination of several of the following: polyacrylate, polyurethane, and organosilicon leveling agents. The thickener is one or a combination of several of the following: a polyurethane or polyacrylate thickener.

7. The method for preparing a self-cleaning, fully shielded infrared and ultraviolet transparent coating according to claim 6, characterized in that... The mass ratio of the dispersant, defoamer, wetting agent, leveling agent and thickener is 1:(0.1~0.3):(0.1~0.2):(0.1~0.2):(0.1~0.2).

8. The method for preparing a self-cleaning, fully shielded infrared and ultraviolet transparent coating according to claim 1, characterized in that... In step three, the mass fraction of the additives in the self-cleaning, fully shielded infrared and ultraviolet transparent coating shall not exceed 5%.

9. The method for preparing a self-cleaning, fully shielded infrared and ultraviolet transparent coating according to claim 1, characterized in that... The molar ratio of tungsten hexachloride to cesium chloride in step (1) ① is 3:(0.5~1); the mass ratio of the total mass of tungsten hexachloride and cesium chloride to citric acid in step (1) ① is (10~20):(20~50); the mass ratio of the total mass of tungsten hexachloride and cesium chloride to polyethylene glycol in step (1) ① is (10~20):(10~30); the heating and stirring temperature in step (1) ① is 60℃~90℃, and the heating and stirring time is 1h~2h; the mass fraction of the ethanol solution in step (2) is 10%~40%; the mass fraction of Na2WO4·2H2O in step (2) is... The volume ratio of the amount to the ethanol solution is (0.5g~1g):50mL; the stirring reaction time in step (3) is 20h~50h; the stirring speed in step (3) is 500r / min~1000r / min; the mass ratio of the nano-cesium tungsten bronze particles to the volume ratio of the reaction solution in step (3) is (0.05g~0.1g):(1mL~3mL); the mass ratio of the WO3-coated nano-cesium tungsten bronze composite material to the volume ratio of the 0.5%~1% octadecyltrichlorosilane anhydrous ethanol solution in step (4) is (1g~3g):(5mL~10mL).

10. The method for preparing a self-cleaning, fully shielded infrared and ultraviolet transparent coating according to claim 1, characterized in that... The ultrasonic dispersion time in step I is 30-60 minutes; the stirring time is 10-20 minutes; the mass-to-volume ratio of nano-indium tin oxide, deionized water, and anhydrous ethanol in step I is (0.5g-1g):(1g-2g):(100mL-200mL); the mass-to-volume ratio of tetrabutyl titanate, polyvinylpyrrolidone, citric acid, oleic acid, stearic acid, and anhydrous ethanol in step I is (15g-20g):(15g-20g):(1g-2g):(1.5g-2g):(10g-25g):(100mL-200mL); the ball milling time in step II is 0.5-1 hour; the cleaning in step II is performed by alternating cleaning with anhydrous ethanol and deionized water, 3-5 times each; the freeze-drying temperature in step II is -45℃ to -55℃, and the freeze-drying time is 20-24 hours.

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