Preparation method of self-adaptive thermal insulation material

By combining GVTO nanomaterials with PVB resin, an adaptive thermal insulation material is formed, which solves the problems of insufficient durability and adaptability of existing thermal insulation materials, and achieves long-lasting thermal insulation performance and simple preparation, making it suitable for fields such as building and automotive glass.

CN120988321APending Publication Date: 2025-11-21NANTONG TONGYI AEROSPACE SCI & TECH CO LTD

Patent Information

Application Number
CN202511409758.5
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-29
Publication Date
2025-11-21

AI Technical Summary

Technical Problem

Existing thermal insulation materials struggle to balance durability, stability, insulation performance, and economic benefits, and lack the ability to adapt to changes in ambient temperature. Furthermore, their manufacturing process is complex and costly.

Method used

By combining GVTO nanomaterials with PVB resin, an adaptive thermal insulation material is formed through spraying and heat treatment, ensuring that the nanomaterials are uniformly dispersed in the resin matrix to form a thin film.

Benefits of technology

It achieves long-lasting thermal insulation performance, adapts to changes in ambient temperature, simplifies the manufacturing process, reduces costs, and is suitable for large-scale production.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a preparation method of a self-adaptive thermal insulation material. When the self-adaptive thermal insulation material is prepared, the preparation method comprises the following steps: preparing a GVTO nano material, carrying out surface modification, carrying out PVB pretreatment, mixing and dispersing, carrying out vacuum defoaming, and coating and heating. The self-adaptive thermal insulation material prepared by the invention can be self-adaptive to environmental temperature change, realizes automatic adjustment of thermal insulation performance, has good mechanical properties and oxygen resistance, is simple and convenient to prepare and is easy for industrial production.
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Description

Technical Field

[0001] This invention relates to the field of thermal insulation materials technology, specifically to a method for preparing an adaptive thermal insulation material. Technical Background

[0002] With increasing awareness of energy consumption and environmental protection, the demand for thermal insulation materials in the construction and automotive industries is growing. An effective thermal insulation material can not only reduce energy consumption and improve living and driving comfort, but also help reduce greenhouse gas emissions. Currently, various thermal insulation materials exist, such as hollow microsphere-modified polymers, glass with specific chemical compositions, and composite films with thermochromic and electrochromic properties. However, a balance between durability, stability, insulation performance, and economic benefits remains a challenge.

[0003] In existing technologies, the use of hollow microspheres to enhance the thermal insulation properties of polymers has been reported. For example, TiO2 and SiO2@TiO2 microspheres have shown good performance in thermal insulation. However, there is still room for improvement in terms of thermal insulation durability and oxygen stability. In addition, the preparation conditions for hollow microspheres are relatively harsh and costly, and the influence of microspheres on polymers is easily limited by the preparation conditions.

[0004] Furthermore, while V2O5-TeO2-P2O5-based glasses exhibit good chemical properties and a low coefficient of thermal expansion, challenges remain in controlling bubble formation within the glass solder. Although PCM composite films possess both thermochromic and electrochromic properties, controlling their phase transition temperature and photoelectric properties presents certain technical challenges. Finally, to address the needs of radiative cooling and summer cooling / winter heating, existing research has proposed the development of temperature-adaptive radiative cooling / photothermal heating materials; however, the sustained performance and self-cleaning properties of these materials still require further improvement.

[0005] Therefore, there is an urgent need to develop a new, cost-effective thermal insulation material, especially one that can adapt to changes in ambient temperature and maintain its insulation effect over a long period of time. Simultaneously, this material should possess good mechanical properties and UV resistance, and its preparation process should be simple and inexpensive to facilitate large-scale application. Summary of the Invention

[0006] The purpose of this invention is to provide a method for preparing an adaptive thermal insulation material to solve the problems existing in the prior art.

[0007] To solve the above-mentioned technical problems, the present invention provides the following technical solution: A method for preparing an adaptive thermal insulation material includes the following steps: (1) Mix ammonium metavanadate solution and tungsten oxide dispersion evenly according to the molar ratio of vanadium and tungsten elements 1:1~2 to obtain vanadium-tungsten mixture. Add 0.1~1% of surfactant by mass of vanadium-tungsten mixture to vanadium-tungsten mixture, adjust pH to 2.8~3.2 with 0.1mol / L hydrochloric acid, place in a reaction vessel, react at 60~120℃ for 6~48h, and dry by spray dryer to obtain GVTO nanomaterials; (2) GVTO nanomaterials, antioxidants and silane hydrolysate are mixed evenly at a mass ratio of 1:0.1~0.2:5~10, ultrasonically treated at 60~70℃ for 6~12h, centrifuged and washed with pure water, and dried to obtain pretreated GVTO nanomaterials; (3) PVB resin and anhydrous ethanol are mixed at a mass ratio of 1:5~10 and stirred at 60~70℃ for 30~40 min. The insoluble impurities are removed by filtration to obtain a PVB resin solution. Under stirring conditions, pretreated GVTO nanomaterials are added to the PVB resin solution at a uniform rate within 30 min. The amount of pretreated GVTO nanomaterials added is 5-10%. After the addition is completed, dispersion treatment is performed to obtain a GVTO dispersion system. After vacuum defoaming of the GVTO dispersion system, it is coated on a substrate and dried in an oven at 70℃ until the solvent is completely evaporated to obtain an adaptive heat insulation material.

[0008] As an optimization, the ammonium metavanadate solution in step (1) is prepared by dissolving ammonium metavanadate in deionized water at 40~60℃.

[0009] As an optimization, the tungsten oxide dispersion in step (1) is prepared by mixing tungsten oxide powder and deionized water at a mass ratio of 1:5~10, followed by ultrasonic dispersion.

[0010] As an optimization, the surfactant in step (1) is one of tetrabutyl titanate and tetraethyl orthosilicate.

[0011] As an optimization, the antioxidant in step (2) is one or a mixture of BASF antioxidant 168, BASF antioxidant 170 and BASF antioxidant 364.

[0012] As an optimization, the silane hydrolysate in step (2) is prepared by mixing silane coupling agent, ethanol and deionized water in a mass ratio of 1:8~10:2~3.

[0013] As an optimization, the silane coupling agent in step (2) is one or a mixture of silane coupling agent KH550, silane coupling agent KH560, and silane coupling agent KH570.

[0014] Compared with the prior art, the beneficial effects achieved by the present invention are: This invention first uses a suitable solvent to dissolve PVB resin, and then adds pre-surface-modified GVTO nanomaterials to the solution. Under specific conditions, high-speed stirring or nano-grinding dispersion treatment is carried out to ensure that the nanomaterials are uniformly dispersed in the resin matrix. Subsequently, the mixed solution is sprayed or coated to form a thin film, and then heat-treated to obtain the final GVTO@PVB adaptive thermal insulation material.

[0015] Compared with existing insulation materials, the GVTO@PVB adaptive thermal insulation material proposed in this invention has significant advantages: First, it breaks through the limitations of traditional materials in terms of thermal insulation performance and durability, possessing a longer service life and superior thermal insulation effect; second, the material's adaptive characteristics mean that it can maintain a relatively constant indoor temperature under different ambient temperatures, greatly improving energy efficiency; finally, the preparation process of GVTO@PVB is simple and easy to carry out, and it is easy to mass-produce, making it highly valuable for industrial applications.

[0016] Accordingly, the GVTO@PVB adaptive thermal insulation material of this invention will significantly improve thermal insulation performance in the fields of automotive and architectural glass, achieving long-term stable performance and having a significant impact on energy conservation, emission reduction, and improvement of the living environment. Furthermore, its adaptive properties and excellent thermal insulation performance can also be applied to a wider range of fields, such as clothing materials, smart home products, and other products requiring thermal insulation, giving this invention a very broad market prospect and social value. Attached Figure Description

[0017] Figure 1 These are electron microscope characterization images of Embodiment 1 of the present invention; Figure 2 Photos taken at the site of the heat insulation test experiment for this invention; Figure 3 This is a graph showing the relationship between infrared irradiation time and indoor center point temperature for Embodiment 1 of the present invention and a commercially available product. Detailed Implementation

[0018] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0019] To more clearly illustrate the method provided by the present invention, the following embodiments will be described in detail.

[0020] The raw materials used in the examples are from the following sources, unless otherwise specified, and are common raw materials in the art: Table 1

[0021] Example 1 A method for preparing an adaptive thermal insulation material mainly includes the following preparation steps: (1) Ammonium metavanadate was dissolved in deionized water at 50℃ to prepare a 0.3 mol / L ammonium metavanadate solution; tungsten oxide powder and deionized water were mixed at a mass ratio of 1:8 and ultrasonically dispersed to prepare a tungsten oxide dispersion; the ammonium metavanadate solution and the tungsten oxide dispersion were mixed evenly at a molar ratio of vanadium to tungsten of 1:1.5 to obtain a vanadium-tungsten mixture; 0.5% tetrabutyl titanate was added to the vanadium-tungsten mixture; the pH was adjusted to 3 with 0.1 mol / L hydrochloric acid; the mixture was placed in a reaction vessel and reacted at 100℃ for 24 h; and then dried by a spray dryer to obtain GVTO nanomaterials. (2) Silane coupling agent KH550, ethanol and deionized water were mixed evenly at a mass ratio of 1:9:2 to prepare silane hydrolysate; GVTO nanomaterials, BASF antioxidant 168 and silane hydrolysate were mixed evenly at a mass ratio of 1:0.1:8, ultrasonically treated at 65℃ for 8h, centrifuged and washed with pure water, and dried to obtain pretreated GVTO nanomaterials; (3) PVB resin and anhydrous ethanol were mixed at a mass ratio of 1:8 and stirred at 65°C for 35 min. The mixture was filtered to remove insoluble impurities and a PVB resin solution was obtained. Under stirring conditions, pretreated GVTO nanomaterials were added to the PVB resin solution at a uniform rate within 30 min. The amount of pretreated GVTO nanomaterials added was 8%. After the addition was completed, the mixture was dispersed to obtain a GVTO dispersion system. The GVTO dispersion system was defoamed under vacuum and then coated onto a substrate. The substrate was dried in an oven at 70°C until the solvent was completely evaporated to obtain an adaptive thermal insulation material.

[0022] Test Example 1 By simulating sunlight with a 275W xenon lamp, the indoor temperature of the 0.76mm thick GVTO@PVB adaptive thermal insulation material obtained in this invention and commercially available products under long-term xenon lamp irradiation was compared. Figure 2 Each test product was attached to a different outer surface of the chamber for testing. The commercially available products used for comparison are from the following sources: Table 2

[0023] The results are as follows: Figure 3 As shown, the film made of the GVTO@PVB adaptive thermal insulation material of the present invention maintains an indoor temperature of approximately 27°C after continuous irradiation for 120 minutes.

[0024] The specific embodiments described above further illustrate the purpose, technical solution, and beneficial effects of the present invention. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for producing a self-adapting thermal insulation material, characterized in that, The method comprises the following steps: (1) uniformly mixing ammonium metavanadate solution and tungsten oxide dispersion liquid according to a molar ratio of vanadium element to tungsten element of 1:1-2 to obtain a vanadium-tungsten mixed solution, adding a surfactant in an amount of 0.1-1% of the mass of the vanadium-tungsten mixed solution to the vanadium-tungsten mixed solution, adjusting the pH to 2.8-3.2 with 0.1 mol / L hydrochloric acid, placing the solution in a reaction kettle, and reacting at 60-120°C for 6-48 h, and drying by a spray dryer to obtain GVTO nanomaterials; (2) uniformly mixing the GVTO nanomaterials, an antioxidant and a silane hydrolysis solution according to a mass ratio of 1:0.1-0.2:5-10, ultrasonically treating at 60-70°C for 6-12 h, centrifugally separating and washing with pure water, and drying to obtain pretreated GVTO nanomaterials; (3) mixing PVB resin and anhydrous ethanol according to a mass ratio of 1:5-10, stirring at 60-70°C for 30-40 min, removing insoluble impurities by filtration to obtain a PVB resin solution; adding the pretreated GVTO nanomaterials to the PVB resin solution at a uniform speed within 30 min under stirring, the addition amount of the pretreated GVTO nanomaterials being 5-10%, and performing dispersion treatment after the addition is completed to obtain a GVTO dispersion system; and coating the GVTO dispersion system on a substrate after vacuum defoaming, drying in an oven at 70°C until the solvent is completely volatilized to obtain a self-adaptive thermal insulation material.

2. The method of claim 1, wherein the self-adapting thermal insulation material is prepared by mixing the first and second materials in a ratio of 1:1 to 1:

3. The ammonium metavanadate solution in step (1) is prepared by dissolving ammonium metavanadate in deionized water at 40-60°C.

3. The method of claim 1, wherein the self-adapting thermal insulation material is prepared by mixing the first and second materials in a ratio of 1:1 to 1:

3. The tungsten oxide dispersion liquid in step (1) is prepared by mixing tungsten oxide powder and deionized water according to a mass ratio of 1:5-10 and ultrasonically dispersing.

4. The method of claim 1, wherein the self-adapting thermal insulation material is prepared by mixing the first and second materials in a ratio of 1:1 to 1:

3. The surfactant in step (1) is one of tetrabutyl titanate and n-silicate.

5. The method of claim 1, wherein the self-adapting thermal insulation material is prepared by mixing the first and second materials in a ratio of 1:1 to 1:

3. The antioxidant in step (2) is one or more of BASF antioxidant 168, BASF antioxidant 170 and BASF antioxidant 364.

6. The method of claim 1, wherein the self-adapting thermal insulation material is prepared by the steps of: The silane hydrolysis solution in step (2) is prepared by uniformly mixing a silane coupling agent, ethanol and deionized water according to a mass ratio of 1:8-10:2-3.

7. The method of claim 6, wherein the self-adapting thermal insulation material is prepared by the steps of: The silane coupling agent in step (2) is one or more of silane coupling agent KH550, silane coupling agent KH560 and silane coupling agent KH570.

Citation Information

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