CN113956702A - Preparation method of in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion liquid - Google Patents
Preparation method of in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion liquid Download PDFInfo
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Abstract
The invention relates to a preparation method of an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion liquid, belonging to the technical field of infrared absorption materials and comprising the following steps of: step 1, weighing tungsten salt and cesium salt according to a certain proportion, dissolving the tungsten salt and the cesium salt in an organic solvent, and preparing cesium-tungsten bronze organic solvent dispersion liquid by using a hydrothermal method; step 2, filtering and emulsifying the cesium tungsten bronze organic solvent dispersion liquid for multiple times to obtain a cesium tungsten bronze aqueous dispersion liquid; and 3, dissolving a titanium salt in the aqueous dispersion, adjusting the pH value of the aqueous solution to 2.5-3.5 by using ammonia water, preserving the temperature for 3-5 h in a closed container at the temperature of 100-120 ℃, and washing to obtain the in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion. According to the preparation method of the in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion liquid, the prepared aqueous dispersion liquid can fully embody the advantages of two materials of cesium tungsten bronze and titanium dioxide.
Description
Technical Field
The invention relates to a preparation method of a cesium tungsten bronze-titanium dioxide aqueous dispersion liquid, in particular to a preparation method of an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion liquid, and belongs to the technical field of infrared absorption materials.
Background
The application of cesium tungsten bronze as an infrared absorption material in many fields has shown unique advantages, and the cesium tungsten bronze is widely used in the fields of transparent heat-insulating glass coatings, solar films, heat-insulating glass laminating films, infrared stealth and the like due to the good visible light transmittance and near-infrared shielding performance of the cesium tungsten bronze.
Chinese patent CN109233362A discloses a cesium tungsten bronze based self-cleaning nano heat insulation coating and a preparation method thereof, wherein cesium tungsten bronze particles are prepared in the first step, titanium dioxide particles are prepared in the second step, and cesium tungsten bronze particles and titanium dioxide particles are mixed and ball-milled to obtain a self-cleaning heat insulation dispersion liquid in the third step.
Disclosure of Invention
The purpose of the invention is: in order to overcome the defects in the prior art, the method for preparing the in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion is provided, and because the titanium dioxide is transparent and is coated on the surface of the cesium tungsten bronze, the infrared absorption function of the cesium tungsten bronze can be ensured, the self-cleaning performance of the titanium dioxide can be fully exerted, and the advantages of two materials of the cesium tungsten bronze and the titanium dioxide can be fully embodied.
The technical scheme for solving the technical problems is as follows:
a preparation method of an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion liquid comprises the following steps:
step 1, weighing tungsten salt and cesium salt according to a certain proportion, dissolving the tungsten salt and the cesium salt in an organic solvent, and performing heat preservation for 10-12 hours in a closed container at 250-300 ℃ by using a hydrothermal method to prepare cesium tungsten bronze organic solvent dispersion liquid;
step 2, filtering the cesium tungsten bronze organic solvent dispersion liquid to obtain a cesium tungsten bronze filter cake, adding water to the cesium tungsten bronze filter cake to emulsify to obtain a cesium tungsten bronze aqueous dispersion liquid, filtering the obtained cesium tungsten bronze aqueous dispersion liquid again to obtain a cesium tungsten bronze filter cake, adding water to emulsify again, and repeating the operation for 3 times to obtain the cesium tungsten bronze aqueous dispersion liquid;
and 3, dissolving a titanium salt in the aqueous dispersion, adjusting the pH value of the aqueous solution to 2.5-3.5 by using ammonia water, preserving the heat for 3-5 h in a closed container at the temperature of 100-120 ℃, and washing to obtain the titanium dioxide coated cesium tungsten bronze-titanium dioxide aqueous dispersion, namely the in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion.
Further, in step 1, the tungsten salt is tungsten chloride, the cesium salt is cesium chloride, and the organic solvent is ethylene glycol or propylene glycol.
Furthermore, the W/Cs molar ratio of the tungsten salt to the cesium salt is 3-5.
Further, in the step 3, the titanium salt is titanyl sulfate, and the molar ratio of Ti/W of the titanium salt to the cesium tungsten bronze aqueous dispersion is 2-3.
Furthermore, in the step 1, the solid content of the cesium tungsten bronze organic solvent dispersion liquid is 15-20%.
Furthermore, in the step 2, the solid content of the cesium tungsten bronze aqueous dispersion liquid is 15-20%.
The invention has the beneficial effects that: the preparation method discloses a preparation method of the in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion for the first time, and the prepared aqueous dispersion is characterized in that the titanium dioxide is transparent and is coated on the surface of the cesium tungsten bronze, so that the infrared absorption function of the cesium tungsten bronze can be ensured, the self-cleaning performance of the titanium dioxide can be fully exerted, and the advantages of two materials of the cesium tungsten bronze and the titanium dioxide can be fully embodied; if the coating is used as an infrared stealth material, the coating can be used as a coating to play an infrared stealth effect, and the coating has a self-cleaning function, so that the effect that the surface of the coating is not required to be cleaned or the cleaning frequency is reduced is achieved; if the material is used as an infrared absorption material, the material can be used for fiber fabrics, can absorb solar infrared rays in alpine regions, achieves the effect of heat preservation and temperature rise after the fabrics absorb heat, achieves the effect of no need of cleaning or reduction of cleaning times due to the self-cleaning function, and solves the problem that the stealth effect of the fiber fabrics is weakened after cleaning.
Drawings
FIG. 1 is an SEM image of an aqueous dispersion of cesium tungsten bronze as described in example 1 of the present invention;
FIG. 2 is an SEM image of an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion as described in example 1 of the present invention;
FIG. 3 is an SEM image of an aqueous dispersion of cesium tungsten bronze as described in example 2 of the present invention;
FIG. 4 is an SEM image of an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion as described in example 2 of the present invention;
FIG. 5 is an SEM image of an aqueous dispersion of cesium tungsten bronze as described in example 3 of the present invention;
fig. 6 is an SEM image of an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion as described in example 3 of the present invention.
Detailed Description
The principles and features of the present invention are described below in conjunction with the accompanying fig. 1-6, which are provided by way of example only to illustrate the present invention and not to limit the scope of the present invention.
Example 1
A preparation method of an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion liquid comprises the following steps:
step 1, accurately weighing 1189.5g of tungsten chloride and 168.5g of cesium chloride, dissolving in a closed container filled with 5433g of ethylene glycol, heating to 250 ℃, and preserving heat for 12 hours to obtain a cesium tungsten bronze ethylene glycol dispersion liquid with the solid content of 15%;
step 2, filtering the cesium tungsten bronze glycol dispersion liquid to obtain a cesium tungsten bronze filter cake, adding water to the cesium tungsten bronze filter cake to emulsify to obtain a cesium tungsten bronze aqueous dispersion liquid, filtering the obtained cesium tungsten bronze aqueous dispersion liquid again to obtain a cesium tungsten bronze filter cake, adding water to emulsify again, repeating the operation for 3 times to obtain a cesium tungsten bronze aqueous dispersion liquid with the solid content of 15%, and performing SEM scanning imaging on the obtained aqueous dispersion liquid, as shown in figure 1;
step 3, weighing 960g of titanyl sulfate, placing the weighed titanyl sulfate in the cesium tungsten bronze aqueous dispersion, adjusting the pH to 2.5 by using ammonia water, preserving the heat for 5 hours in a closed container at 100 ℃, naturally cooling to obtain an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion, and carrying out SEM scanning imaging on the obtained aqueous dispersion as shown in figure 2.
Example 2
A preparation method of an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion liquid comprises the following steps:
step 1, accurately weighing 991.5g of tungsten chloride and 84.5g of cesium chloride, dissolving the tungsten chloride and the cesium chloride in a closed container filled with 2700g of propylene glycol, heating to 300 ℃, and preserving heat for 10 hours to obtain a cesium tungsten bronze propylene glycol dispersion liquid with the solid content of 20%;
step 2, filtering the cesium tungsten bronze propylene glycol dispersion liquid to obtain a cesium tungsten bronze filter cake, adding water to the cesium tungsten bronze filter cake to emulsify to obtain a cesium tungsten bronze aqueous dispersion liquid, filtering the obtained cesium tungsten bronze aqueous dispersion liquid again to obtain a cesium tungsten bronze filter cake, adding water to emulsify again, repeating the operation for 3 times to obtain a cesium tungsten bronze aqueous dispersion liquid with the solid content of 20%, and performing SEM scanning imaging on the obtained aqueous dispersion liquid, as shown in FIG. 3;
step 3, weighing 800g of titanyl sulfate, placing the weighed titanyl sulfate in the cesium tungsten bronze aqueous dispersion, adjusting the pH to 3.5 by using ammonia water, preserving the heat in a closed container at 120 ℃ for 3h, naturally cooling to obtain an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion, and carrying out SEM scanning imaging on the obtained aqueous dispersion as shown in figure 4.
Example 3
A preparation method of an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion liquid comprises the following steps:
step 1, accurately weighing 796.5g of tungsten chloride and 84.5g of cesium chloride, dissolving in a closed container filled with 2487g of propylene glycol, heating to 280 ℃, and preserving heat for 11 hours to obtain cesium tungsten bronze propylene glycol dispersion liquid with the solid content of 18%;
step 2, filtering the cesium tungsten bronze propylene glycol dispersion liquid to obtain a cesium tungsten bronze filter cake, adding water to the cesium tungsten bronze filter cake to emulsify to obtain a cesium tungsten bronze aqueous dispersion liquid, filtering the obtained cesium tungsten bronze aqueous dispersion liquid again to obtain a cesium tungsten bronze filter cake, adding water to emulsify again, repeating the operation for 3 times to obtain a cesium tungsten bronze aqueous dispersion liquid with the solid content of 17%, and performing SEM scanning imaging on the obtained aqueous dispersion liquid, as shown in FIG. 5;
step 3, weighing 803g of titanyl sulfate, placing the weighed titanyl sulfate in the cesium tungsten bronze aqueous dispersion, adjusting the pH value to 3.0 by using ammonia water, preserving the heat for 4 hours in a closed container at the temperature of 110 ℃, naturally cooling to obtain an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion, and carrying out SEM scanning imaging on the obtained aqueous dispersion as shown in figure 6.
Comparing the SEM images in the various examples, the conclusion is as follows: in three examples, the in situ titanium dioxide modified cesium tungsten bronze surface was coated with a titanium dioxide layer, consistent with the expectations of the preparation method.
The preparation method discloses a preparation method of the in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion for the first time, and the prepared aqueous dispersion is characterized in that the titanium dioxide is transparent and is coated on the surface of the cesium tungsten bronze, so that the infrared absorption function of the cesium tungsten bronze can be ensured, the self-cleaning performance of the titanium dioxide can be fully exerted, and the advantages of two materials of the cesium tungsten bronze and the titanium dioxide can be fully embodied; if the coating is used as an infrared stealth material, the coating can be used as a coating to play an infrared stealth effect, and the coating has a self-cleaning function, so that the effect that the surface of the coating is not required to be cleaned or the cleaning frequency is reduced is achieved; if the material is used as an infrared absorption material, the material can be used for fiber fabrics, can absorb solar infrared rays in alpine regions, achieves the effect of heat preservation and temperature rise after the fabrics absorb heat, achieves the effect of no need of cleaning or reduction of cleaning times due to the self-cleaning function, and solves the problem that the stealth effect of the fiber fabrics is weakened after cleaning.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (6)
1. The preparation method of the in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion is characterized by comprising the following steps of:
step 1, weighing tungsten salt and cesium salt according to a certain proportion, dissolving the tungsten salt and the cesium salt in an organic solvent, and performing heat preservation for 10-12 hours in a closed container at 250-300 ℃ by using a hydrothermal method to prepare cesium tungsten bronze organic solvent dispersion liquid;
step 2, filtering the cesium tungsten bronze organic solvent dispersion liquid to obtain a cesium tungsten bronze filter cake, adding water to the cesium tungsten bronze filter cake to emulsify to obtain a cesium tungsten bronze aqueous dispersion liquid, filtering the obtained cesium tungsten bronze aqueous dispersion liquid again to obtain a cesium tungsten bronze filter cake, adding water to emulsify again, and repeating the operation for 3 times to obtain the cesium tungsten bronze aqueous dispersion liquid;
and 3, dissolving a titanium salt in the aqueous dispersion, adjusting the pH value of the aqueous solution to 2.5-3.5 by using ammonia water, preserving the heat for 3-5 h in a closed container at the temperature of 100-120 ℃, and washing to obtain the titanium dioxide coated cesium tungsten bronze-titanium dioxide aqueous dispersion, namely the in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion.
2. The method of preparing an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion according to claim 1, characterized in that: in the step 1, the tungsten salt is tungsten chloride, the cesium salt is cesium chloride, and the organic solvent is ethylene glycol or propylene glycol.
3. The method of preparing an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion according to claim 2, characterized in that: the W/Cs molar ratio of the tungsten salt to the cesium salt is 3-5.
4. The method of preparing an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion according to claim 1, characterized in that: in the step 3, the titanium salt is titanyl sulfate, and the molar ratio of Ti/W of the titanium salt to the cesium tungsten bronze aqueous dispersion is 2-3.
5. The method of preparing an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion according to claim 1, characterized in that: in the step 1, the solid content of the cesium tungsten bronze organic solvent dispersion liquid is 15-20%.
6. The method of preparing an in-situ coated cesium tungsten bronze-titanium dioxide aqueous dispersion according to claim 5, characterized in that: in the step 2, the solid content of the cesium tungsten bronze aqueous dispersion liquid is 15-20%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449254A (en) * | 2022-09-22 | 2022-12-09 | 华南理工大学 | Cesium tungsten bronze/silicon dioxide hollow microsphere composite material and preparation method and application thereof |
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| US20180340082A1 (en) * | 2017-05-25 | 2018-11-29 | The Hong Kong Polytechnic University | Cesium tungsten bronze-based self-cleaning nano heat-insulation coating material and preparation method thereof |
| CN113185871A (en) * | 2021-04-14 | 2021-07-30 | 华南理工大学 | Tungsten bronze-based super-hydrophobic transparent heat-insulating coating and preparation method thereof |
| CN113249091A (en) * | 2021-05-19 | 2021-08-13 | 东北大学秦皇岛分校 | ATO (antimony tin oxide) coated cesium tungsten bronze composite nano powder and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20180340082A1 (en) * | 2017-05-25 | 2018-11-29 | The Hong Kong Polytechnic University | Cesium tungsten bronze-based self-cleaning nano heat-insulation coating material and preparation method thereof |
| CN109233362A (en) * | 2017-05-25 | 2019-01-18 | 香港理工大学 | A kind of self-cleaning nona insulating moulding coating and preparation method thereof based on caesium tungsten bronze |
| CN107513293A (en) * | 2017-08-10 | 2017-12-26 | 广州市黑本新材料科技有限公司 | A kind of preparation method of caesium tungsten bronze modified powder and its slurry |
| CN113185871A (en) * | 2021-04-14 | 2021-07-30 | 华南理工大学 | Tungsten bronze-based super-hydrophobic transparent heat-insulating coating and preparation method thereof |
| CN113249091A (en) * | 2021-05-19 | 2021-08-13 | 东北大学秦皇岛分校 | ATO (antimony tin oxide) coated cesium tungsten bronze composite nano powder and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115449254A (en) * | 2022-09-22 | 2022-12-09 | 华南理工大学 | Cesium tungsten bronze/silicon dioxide hollow microsphere composite material and preparation method and application thereof |
| CN115449254B (en) * | 2022-09-22 | 2023-08-04 | 华南理工大学 | Cesium tungsten bronze/silicon dioxide hollow microsphere composite material and preparation method and application thereof |
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Application publication date: 20220121 |