CN119192918B - Preparation method of near infrared shielding coating with high visible light transmittance - Google Patents
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Abstract
本发明适用于玻璃透明隔热涂层技术领域，一种高可见光透过率的近红外屏蔽涂层的制备方法，其包括以下步骤：将浓度为1‑10%的HxWO3·2H2O蓝色粉末溶液与聚乙烯醇缩丁醛酯粉末按照质量比为1：5‑10充分混合，得到浆料，接着将所述浆料旋涂法涂覆于玻璃样品表面上，最后干燥，得到玻璃涂层。有益效果：本发明公开了一种高可见光透过率的近红外屏蔽涂层的制备方法，不仅具有优良的近红外屏蔽特性，而且在可见光区的透过率显著优于铯钨青铜涂层，紫外线屏敝率比铯钨青铜更高，其中制备HxWO3·2H2O蓝色粉末溶液的方法简单，易操作，耗时少，成本低，适合大规模生产。
The present invention is applicable to the technical field of glass transparent heat-insulating coatings, and is a method for preparing a near-infrared shielding coating with high visible light transmittance, which comprises the following steps: a 1-10% HxWO 3 ·2H 2 O blue powder solution is fully mixed with polyvinyl butyral ester powder in a mass ratio of 1:5-10 to obtain a slurry, and then the slurry is applied on the surface of a glass sample by spin coating, and finally dried to obtain a glass coating. Beneficial effects: The present invention discloses a method for preparing a near-infrared shielding coating with high visible light transmittance, which not only has excellent near-infrared shielding properties, but also has a transmittance in the visible light region that is significantly better than that of a cesium tungsten bronze coating, and a higher ultraviolet shielding rate than that of cesium tungsten bronze, wherein the method for preparing the HxWO 3 ·2H 2 O blue powder solution is simple, easy to operate, less time-consuming, low-cost, and suitable for large-scale production.
Description
Technical Field
The invention relates to the technical field of glass transparent heat-insulating coatings, in particular to a preparation method of a near infrared shielding coating with high visible light transmittance.
Background
The contribution of near infrared light in the heat radiation energy of solar spectrum is close to 50%, and a large amount of refrigeration energy is consumed for buildings or vehicles by the heat radiation in hot summer, so that the development of the transparent heat insulation material for the windows with low cost and high performance and the coating thereof has great economic and social benefits and excellent development prospect. At present, a tungsten bronze material is an excellent near infrared shielding material, wherein cesium or sodium and other alkali metal tungsten bronze is excellent in terms of visible light transmittance and near infrared shielding performance, and therefore, the tungsten bronze material is widely applied in the field of transparent heat insulation films. The application number CN201910699087.9 discloses a method for preparing cesium tungsten bronze material at normal pressure, which takes tungsten hexachloride as tungsten source and cesium hydroxide as cesium source under the conditions of normal pressure and 40-78 ℃, the application number CN202311523822.3 discloses a method for preparing superfine cesium tungsten bronze powder, which comprises the steps of mixing tungsten source, cesium source and organic solvent, preserving heat at 80-150 ℃ and then reacting at 100-300 ℃ to obtain cesium tungsten bronze powder, wherein the above patent discloses synthesized cesium tungsten bronze which has excellent near infrared shielding performance and better visible light transmittance but still does not meet the requirements of scenes with high visible light transmittance, such as front windshield of an automobile. In order to solve the technical shortboard, the application provides a preparation method of a near infrared shielding coating with high visible light transmittance, the prepared hydrogen tungsten bronze hydrate coating not only has excellent near infrared shielding property, but also has obviously better transmittance in the visible light region than cesium tungsten bronze coating, and has higher ultraviolet shielding rate than cesium tungsten bronze.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method of a near infrared shielding coating which has excellent near infrared shielding characteristics and is suitable for large-scale production and high in visible light transmittance.
The preparation method of the near infrared shielding coating with high visible light transmittance comprises the following steps of fully mixing H xWO3·2H2 O blue powder solution with concentration of 1-10% and polyvinyl butyral powder according to mass ratio of 1:5-10 to obtain slurry, then coating the slurry on the surface of a glass sample by a spin coating method, and finally drying to obtain the glass coating, wherein x is more than or equal to 0 and less than or equal to 1.
Further, the granularity of the H xWO3·2H2 O blue powder is 5-100nm.
Further, the preparation method of the H xWO3·2H2 O blue powder solution comprises the following steps:
(1) Pretreatment, namely stirring and mixing LaO 3H3 powder and benzyl alcohol according to the mass ratio of 1:500-1000, and stirring until LaO 3H3 powder is completely dissolved to obtain LaO 3H3 solution;
(2) Preparing a precursor solution, namely mixing the LaO 3H3 solution in the step (1) with WCl 6 raw materials according to the mass ratio of 20-40:1, and stirring and mixing by magnetic force to obtain the precursor solution;
(3) The precursor solution in the step (2) is placed in a reaction kettle, the reaction kettle is placed in a microwave synthesizer, the reaction is carried out under the combined action of hydrothermal and microwaves, the reaction temperature is 50-200 ℃, the reaction time is 5-240min, and then the reaction kettle is naturally cooled to room temperature, so that a reaction solution is obtained;
(4) And (3) separating and washing, namely centrifugally separating the reaction solution in the step (3), and washing the separated solid by deionized water, absolute ethyl alcohol, dilute sulfuric acid, ionized water and absolute ethyl alcohol in sequence to obtain the H xWO3·2H2 O blue powder solution.
Further, the stirring condition in the step (1) is that the stirring speed is 100-800r/min. Too low stirring speed leads to uneven mixing of the solution, insufficient contact between LaO 3H3 and WCl 6, influences the reaction rate and the morphology of the product, too high stirring speed can cause excessive evaporation or local overheating of the solvent, further influences the quality of the product, too short stirring time can lead to incomplete mixing of the precursor solution, insufficient reaction, poor crystallinity, uneven particle size or low yield of the reaction product, too long stirring time can lead to evaporation of the solvent, or increase the risk of mechanical damage, and the stability of the reaction system is reduced.
Further, the stirring condition in the step (2) is that the stirring speed is 100-800r/min and the stirring time is 10-60min.
Further, the centrifugal separation condition in the step (4) is that the rotating speed is 3000-5000r/min and the time is 2-10min. Too low a centrifugation speed may not effectively separate the precipitate, resulting in incomplete washing processes, possibly causing residual solvents or reaction byproducts to affect subsequent reactions and purity of the particles, too high a centrifugation speed may cause agglomeration of the particles, affecting final particle size and distribution, too short a centrifugation time may cause insufficient sedimentation of the solids, affecting subsequent washing efficiency, thereby failing to effectively remove impurities in the solvent, too long a centrifugation time may cause compaction or agglomeration of the solid particles, difficult redispersion or affecting particle morphology.
Further, the method for washing the ionized water in the step (4) comprises the steps of washing the separated solid and deionized water in an ultrasonic cleaner for 5-30min, and then putting the solid and the deionized water into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
Further, the method for washing the absolute ethyl alcohol in the step (4) comprises the steps of washing the separated solid and the absolute ethyl alcohol in an ultrasonic cleaner for 5-30min, and then putting the solid and the absolute ethyl alcohol into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
Further, the method for washing the dilute sulfuric acid in the step (4) comprises the steps of washing the separated solid and the dilute sulfuric acid with the concentration of 20-30% in an ultrasonic cleaner for 5-30min, and then putting the solid and the dilute sulfuric acid into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
The invention has the advantages that:
1. The invention discloses a preparation method of a near infrared shielding coating with high visible light transmittance, which comprises the steps of mixing H xWO3·2H2 O blue powder solution with polyvinyl butyral powder, and coating the mixture on the surface of a glass sample to form a hydrogen tungsten bronze hydrate glass coating, wherein the hydrogen tungsten bronze hydrate glass coating not only has excellent near infrared shielding property, but also has the transmittance in a visible light region obviously superior to that of a cesium tungsten bronze coating, and the shielding rate of ultraviolet rays is also superior to that of the cesium tungsten bronze coating.
2. The invention discloses a preparation method of a near infrared shielding coating with high visible light transmittance, wherein the method for preparing H xWO3·2H2 O blue powder solution is simple, easy to operate, less in time consumption and low in cost, is suitable for large-scale production, and the prepared H xWO3·2H2 O blue powder solution can be directly mixed with polyvinyl butyral powder without drying for coating glass, so that the preparation method is convenient to use.
Drawings
FIG. 1 is an XRD pattern of H xWO3·2H2 O blue powder according to example 1 of the present invention;
FIG. 2 is an SEM image of H xWO3·2H2 O blue powder according to example 1 of the present invention;
FIG. 3 is a graph showing transmittance of glass coatings of example 1 and comparative example 1 of the present invention.
Detailed Description
It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other. The application will be described in detail below with reference to the drawings in connection with embodiments.
It is noted that all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs unless otherwise indicated.
In the present invention, unless otherwise indicated, the terms "upper" and "lower" are used generally in the directions shown in the drawings or in the vertical, vertical or gravitational directions, and similarly, for convenience of understanding and description, the terms "left" and "right" are used generally in the directions shown in the drawings, and the terms "inner" and "outer" are used to refer to the inner and outer sides with respect to the outline of each component itself, but the terms of orientation are not intended to limit the present invention.
Example 1A method for preparing a near infrared shielding coating with high visible light transmittance, comprising the steps of thoroughly mixing 100mL of H xWO3·2H2 O blue powder solution with concentration of 5% with 37.5g of polyvinyl butyral ester powder to obtain slurry, then coating the slurry on the surface of a glass sample by a spin coating method, and finally drying to obtain the glass coating, wherein x is more than or equal to 0 and less than or equal to 1. Wherein the granularity of the H xWO3·2H2 O blue powder is 5-100nm.
The preparation method of the H xWO3·2H2 O blue powder solution comprises the following steps:
(1) Pretreatment, namely stirring and mixing 0.0779 g LaO 3H3 powder and 50ml benzyl alcohol until the LaO 3H3 powder is completely dissolved to obtain LaO 3H3 solution, wherein the stirring speed is 100-800r/min.
(2) Preparing a precursor solution, namely mixing the LaO 3H3 solution in the step (1) with 1.6260g of WCl 6 raw material, and stirring and mixing by magnetic force to obtain the precursor solution, wherein the stirring speed is 100-800r/min, and the stirring time is 10-60min.
(3) The precursor solution in the step (2) is placed in a reaction kettle, the reaction kettle is placed in a microwave synthesizer, the reaction is carried out under the combined action of hydrothermal and microwaves, the reaction temperature is 50-200 ℃, the reaction time is 5-240min, and then the reaction solution is obtained after natural cooling to room temperature;
(4) And (3) separating and washing, namely centrifugally separating the reaction solution in the step (3), wherein the rotating speed is 3000-5000r/min, and the time is 2-10min, and washing the separated solid by deionized water, absolute ethyl alcohol, dilute sulfuric acid, ionized water and absolute ethyl alcohol in sequence to obtain H xWO3·2H2 O blue powder solution. The powder was analyzed by an X-ray diffractometer, and the results are shown in fig. 1. As can be seen from FIG. 1, the diffraction peak position of the obtained powder is well matched with that of a standard Card PDF Card of H 0.12WO3·2H2 O, namely 40-0693, and the microstructure of the powder is observed through a Scanning Electron Microscope (SEM), and the result is shown in FIG. 2. As is clear from FIG. 2, the H xWO3·2H2 O blue powder obtained in example 1 had a uniform particle size distribution and excellent dispersibility, and the particle size distribution was 10-40nm.
The method for washing with ionized water comprises the steps of washing the separated solid and deionized water in an ultrasonic cleaner for 5-30min, and centrifuging in a centrifuge with the rotating speed of 3000-5000r/min for 2-10min.
The method for washing the absolute ethyl alcohol specifically comprises the steps of washing the solid after washing and separating by using ionized water and the absolute ethyl alcohol in an ultrasonic cleaner for 5-30min, and then putting the solid and the absolute ethyl alcohol into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
The method for washing the dilute sulfuric acid comprises the steps of washing the solid washed and separated by absolute ethyl alcohol and the dilute sulfuric acid with the concentration of 20-30% in an ultrasonic cleaner for 5-30min, and then putting the solid into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
The method for preparing the H xWO3·2H2 O blue powder solution is simple, easy to operate, less in time consumption, low in cost and suitable for large-scale production, and the prepared H xWO3·2H2 O blue powder solution can be directly mixed with polyvinyl butyral powder without drying for coating glass, so that the method is convenient to use.
Example 2A method for preparing a near infrared shielding coating with high visible light transmittance, comprising the steps of thoroughly mixing 100mL of H xWO3·2H2 O blue powder solution with concentration of 1% with 5g of polyvinyl butyral ester powder to obtain slurry, then coating the slurry on the surface of a glass sample by a spin coating method, and finally drying to obtain the glass coating, wherein x is more than or equal to 0 and less than or equal to 1. Wherein the granularity of the H xWO3·2H2 O blue powder is 5-100nm.
The preparation method of the H xWO3·2H2 O blue powder solution comprises the following steps:
(1) Pretreatment, namely stirring and mixing 0.2000g of LaO 3H3 powder with 100mL of benzyl alcohol until the LaO 3H3 powder is completely dissolved to obtain LaO 3H3 solution, wherein the stirring speed is 100-800r/min.
(2) Preparing a precursor solution, namely mixing the LaO 3H3 solution in the step (1) with 5.0100g of WCl 6 raw material, and stirring and mixing by magnetic force to obtain the precursor solution, wherein the stirring speed is 100-800r/min, and the stirring time is 10-60min.
(3) The precursor solution in the step (2) is placed in a reaction kettle, the reaction kettle is placed in a microwave synthesizer, the reaction is carried out under the combined action of hydrothermal and microwaves, the reaction temperature is 50-200 ℃, the reaction time is 5-240min, and then the reaction solution is obtained after natural cooling to room temperature;
(4) And (3) separating and washing, namely centrifugally separating the reaction solution in the step (3), wherein the rotating speed is 3000-5000r/min, and the time is 2-10min, and washing the separated solid by deionized water, absolute ethyl alcohol, dilute sulfuric acid, ionized water and absolute ethyl alcohol in sequence to obtain H xWO3·2H2 O blue powder solution.
The method for washing with ionized water comprises the steps of washing the separated solid and deionized water in an ultrasonic cleaner for 5-30min, and centrifuging in a centrifuge with the rotating speed of 3000-5000r/min for 2-10min.
The method for washing the absolute ethyl alcohol specifically comprises the steps of washing the solid after washing and separating by using ionized water and the absolute ethyl alcohol in an ultrasonic cleaner for 5-30min, and then putting the solid and the absolute ethyl alcohol into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
The method for washing the dilute sulfuric acid comprises the steps of washing the solid washed and separated by absolute ethyl alcohol and the dilute sulfuric acid with the concentration of 20-30% in an ultrasonic cleaner for 5-30min, and then putting the solid into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
The method for preparing the H xWO3·2H2 O blue powder solution is simple, easy to operate, less in time consumption, low in cost and suitable for large-scale production, and the prepared H xWO3·2H2 O blue powder solution can be directly mixed with polyvinyl butyral powder without drying for coating glass, so that the method is convenient to use.
Example 3A method for preparing a near infrared shielding coating with high visible light transmittance, comprising the steps of thoroughly mixing 100mL of H xWO3·2H2 O blue powder solution with concentration of 10% with 10g of polyvinyl butyral ester powder to obtain slurry, then coating the slurry on the surface of a glass sample by a spin coating method, and finally drying to obtain the glass coating, wherein x is more than or equal to 0 and less than or equal to 1. Wherein the granularity of the H xWO3·2H2 O blue powder is 5-100nm.
The preparation method of the H xWO3·2H2 O blue powder solution comprises the following steps:
(1) Pretreatment, namely stirring and mixing 0.1500g of LaO 3H3 powder with 150mL of benzyl alcohol, and stirring until the LaO 3H3 powder is completely dissolved to obtain LaO 3H3 solution, wherein the stirring speed is 100-800r/min.
(2) Preparing a precursor solution, namely mixing the LaO 3H3 solution in the step (1) with 3.7537g of WCl 6 raw material, and stirring and mixing by magnetic force to obtain the precursor solution, wherein the stirring speed is 100-800r/min, and the stirring time is 10-60min.
(3) The precursor solution in the step (2) is placed in a reaction kettle, the reaction kettle is placed in a microwave synthesizer, the reaction is carried out under the combined action of hydrothermal and microwaves, the reaction temperature is 50-200 ℃, the reaction time is 5-240min, and then the reaction solution is obtained after natural cooling to room temperature;
(4) And (3) separating and washing, namely centrifugally separating the reaction solution in the step (3), wherein the rotating speed is 3000-5000r/min, and the time is 2-10min, and washing the separated solid by deionized water, absolute ethyl alcohol, dilute sulfuric acid, ionized water and absolute ethyl alcohol in sequence to obtain H xWO3·2H2 O blue powder solution.
The method for washing with ionized water comprises the steps of washing the separated solid and deionized water in an ultrasonic cleaner for 5-30min, and centrifuging in a centrifuge with the rotating speed of 3000-5000r/min for 2-10min.
The method for washing the absolute ethyl alcohol specifically comprises the steps of washing the solid after washing and separating by using ionized water and the absolute ethyl alcohol in an ultrasonic cleaner for 5-30min, and then putting the solid and the absolute ethyl alcohol into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
The method for washing the dilute sulfuric acid comprises the steps of washing the solid washed and separated by absolute ethyl alcohol and the dilute sulfuric acid with the concentration of 20-30% in an ultrasonic cleaner for 5-30min, and then putting the solid into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
The method for preparing the H xWO3·2H2 O blue powder solution is simple, easy to operate, less in time consumption, low in cost and suitable for large-scale production, and the prepared H xWO3·2H2 O blue powder solution can be directly mixed with polyvinyl butyral powder without drying for coating glass, so that the method is convenient to use.
Comparative example 1 0.377 grams of CsOH ∙ H 2 O and 150mL of benzyl alcohol solution were mixed with stirring for 20 minutes, then 0.9 grams of WCl 6 were added to maintain a concentration of WCl 6 in the precursor solution of 0.015M. The solution was then transferred to an autoclave and reacted at 200 ℃ for 4 hours. Finally, washing the product with deionized water and alcohol for multiple times to obtain cesium tungsten bronze Cs 0.33WO3 solution, adding 37.5g of polyvinyl butyral ester powder into the solution, fully mixing to obtain slurry, then coating the slurry on the surface of a glass sample by a spin coating method, and finally drying to obtain the glass coating.
Experiments the glass coatings prepared in example 1 and comparative example 1 were subjected to transmittance test using an ultraviolet-visible-near infrared photometer (instrument model: UH 4150), and as shown in FIG. 3, it can be seen from FIG. 3 that the glass coating prepared in example 1 has a wider transmittance in the visible region and a lower transmittance in the ultraviolet region of 400nm or less than that in comparative example 1, relative to that in comparative example 1. Therefore, compared with cesium tungsten bronze coating, the H xWO3·2H2 O glass coating prepared by the method has better visible light transmittance and ultraviolet shielding rate on the premise of ensuring better near infrared shielding rate.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
The above description is only a preferred embodiment of the present invention, and the protection scope of the present invention is not limited to the above examples, and all technical solutions belonging to the concept of the present invention belong to the protection scope of the present invention. It should be noted that modifications and adaptations to the present invention may occur to one skilled in the art without departing from the principles of the present invention and are intended to be within the scope of the present invention.
Claims (7)
1. The preparation method of the near infrared shielding coating with high visible light transmittance is characterized by comprising the following steps of fully mixing H xWO3·2H2 O blue powder solution with the concentration of 1-10% with polyvinyl butyral ester powder according to the mass ratio of 1:5-10 to obtain slurry, then coating the slurry on the surface of a glass sample by a spin coating method, and finally drying to obtain the glass coating, wherein x is more than or equal to 0 and less than or equal to 1;
the preparation method of the H xWO3·2H2 O blue powder solution comprises the following steps:
(1) Pretreatment, namely stirring and mixing LaO 3H3 powder and benzyl alcohol according to the mass ratio of 1:500-1000, and stirring until LaO 3H3 powder is completely dissolved to obtain LaO 3H3 solution;
(2) Preparing a precursor solution, namely mixing the LaO 3H3 solution in the step (1) with WCl 6 raw materials according to the mass ratio of 20-40:1, and stirring and mixing by magnetic force to obtain the precursor solution;
(3) The precursor solution in the step (2) is placed in a reaction kettle, the reaction kettle is placed in a microwave synthesizer, the reaction is carried out under the combined action of hydrothermal and microwaves, the reaction temperature is 50-200 ℃, the reaction time is 5-240min, and then the reaction kettle is naturally cooled to room temperature, so that a reaction solution is obtained;
(4) And (3) separating and washing, namely centrifugally separating the reaction solution in the step (3), and sequentially washing the separated solid by deionized water, absolute ethyl alcohol, dilute sulfuric acid, ionized water and absolute ethyl alcohol to obtain the H xWO3·2H2 O blue powder solution, wherein the granularity of the H xWO3·2H2 O blue powder is 5-100nm.
2. The method for producing a near infrared shielding coating having a high visible light transmittance according to claim 1, wherein the stirring condition in the step (1) is a stirring speed of 100 to 800r/min.
3. The method for producing a near infrared shielding coating having a high visible light transmittance according to claim 1, wherein the stirring condition in the step (2) is a stirring speed of 100 to 800r/min and a stirring time of 10 to 60min.
4. The method for preparing the near infrared shielding coating with high visible light transmittance according to claim 1, wherein the centrifugal separation condition in the step (4) is that the rotating speed is 3000-5000r/min and the time is 2-10min.
5. The method for preparing the near infrared shielding coating with high visible light transmittance according to claim 1, wherein the method for washing with ionized water in the step (4) is characterized in that the separated solid and deionized water are washed in an ultrasonic cleaner for 5-30min, and then are put into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
6. The method for preparing the near infrared shielding coating with high visible light transmittance according to claim 1, wherein the method for washing the absolute ethyl alcohol in the step (4) is characterized in that the separated solid and the absolute ethyl alcohol are washed for 5-30min in an ultrasonic cleaner, and then are put into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
7. The method for preparing the near infrared shielding coating with high visible light transmittance according to claim 1, wherein the method for washing the dilute sulfuric acid in the step (4) is characterized in that the separated solid and the dilute sulfuric acid with the concentration of 20-30% are washed for 5-30min in an ultrasonic cleaner, and then are put into a centrifuge with the rotating speed of 3000-5000r/min for centrifugation for 2-10min.
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