Alumina aerogel composite starting material composition, alumina aerogel composite, and method of making the same

Abstract

The application provides an alumina aerogel composite raw material composition, an alumina aerogel composite and a preparation method thereof. The alumina aerogel composite raw material composition comprises an alumina aerogel and a high-temperature-resistant resin raw material composition, and the high-temperature-resistant resin raw material composition comprises a high-temperature-resistant resin and an aprotic solvent. By using the high-temperature-resistant resin, the technical scheme of the application can significantly improve the compression performance of the alumina aerogel, while maintaining the high-temperature resistance and heat insulation performance of the alumina aerogel. The high-temperature-resistant alumina aerogel composite heat insulation material prepared by using the raw material composition has a temperature resistance of greater than or equal to 1000 DEG C. The alumina aerogel composite raw material composition provided by the application can obtain the high-temperature-resistant alumina aerogel composite heat insulation material with high compression strength through only two steps of impregnation and curing, and is convenient to use.

Description

Technical Field

[0001] This invention relates to the field of aerogel composite materials technology, and more specifically, to an alumina aerogel composite material raw material composition, an alumina aerogel composite material, and a method for preparing the same. Background Technology

[0002] Alumina, due to its advantages such as high temperature resistance, corrosion resistance, good thermal insulation, high electrical insulation, stable chemical properties, and low cost, is widely used as a high-temperature insulation material in defense, aerospace, high-temperature thermal protective clothing, and high-temperature boilers. Alumina aerogel materials, with their micro- and nano-porous structures, achieve equivalent thermal insulation effects with lighter weight and smaller volume. They are suitable for applications such as thermal insulation materials for aero-engines, space exploration vehicles, and transportation vehicles, offering excellent thermal insulation while reducing overall weight, showing great promise for future applications. Furthermore, due to its stable chemical properties and high porosity, high specific surface area, and open textured structure, alumina aerogel has potential applications as a catalyst and catalyst support.

[0003] Due to the weak inter-fiber forces in alumina aerogel, its compressive strength is low, leading to a "flaking" phenomenon in practical applications. This makes it unsuitable for applications with significant impact loads, such as aerospace engines, high-speed aircraft thermal protection systems, tank armor, and high-temperature thermal protection. Therefore, improving the mechanical strength of alumina aerogel has received considerable attention. For example, patent (CN 105601309 B) uses inorganic fibers such as carbon fiber or silicon carbide fiber to enhance the flexural strength and toughness of alumina aerogel. However, because these are inorganic materials, the weak inter-fiber forces still inevitably result in the "flaking" problem. Using organic materials to fix the overlapping nodes between the alumina aerogel fibers can significantly improve its compressive strength; however, ordinary organic materials are not heat-resistant and cannot maintain the high-temperature resistance of alumina aerogel. Summary of the Invention

[0004] The main objective of this invention is to provide an alumina aerogel composite material raw material composition, an alumina aerogel composite material, and a method for preparing the same, in order to solve the problems of low compressive strength and easy "flaking" of alumina aerogel materials in the prior art.

[0005] To achieve the above objectives, according to one aspect of the present invention, an alumina aerogel composite material composition is provided, the composition comprising alumina aerogel and a high-temperature resistant resin material composition, wherein the high-temperature resistant resin material composition comprises a high-temperature resistant resin and an aprotic solvent.

[0006] Furthermore, the high-temperature resistant resin raw materials include high-temperature resistant resin, aluminum silver powder, aprotic solvent, anti-settling agent, coupling agent and dispersant;

[0007] Preferably, by weight, the high-temperature resistant resin raw material includes 10-50 parts of high-temperature resistant resin, 6-16 parts of aluminum silver powder, 30-85 parts of aprotic solvent, 1-7 parts of anti-settling agent, 0.01-5 parts of coupling agent and 0.01-5 parts of dispersant.

[0008] Furthermore, the high-temperature resistant resin includes any one or more of KB-8812, KB-8124, KB-8813 and KB-8124S.

[0009] Furthermore, the alumina aerogel includes alumina fibers, the average diameter of which is 1-30 μm, preferably 3-20 μm;

[0010] Preferably, the density of the alumina aerogel is 0.05-1 g / cm³. 3 Preferably, it is 0.1-0.6 g / cm³. 3 .

[0011] Furthermore, the aprotic solvent includes any one or more selected from dimethylformamide, dimethylacetamide, dimethyl sulfoxide, and n-butyl acetate.

[0012] Furthermore, the anti-settling agent includes any one or more selected from 201 anti-settling agent, fumed SiO2, high clay and talc.

[0013] Furthermore, the coupling agent includes any one or more selected from KH-560, KH-550 and KH-570;

[0014] And / or, the dispersant includes any one or more selected from 232S dispersant, BYK-9076, BYK-171, BYK-174 and BYK-112.

[0015] According to another aspect of this application, a method for preparing an alumina aerogel composite material is provided. The method includes: step S1, mixing any of the above-mentioned high-temperature resistant resin raw materials and stirring evenly to obtain a high-temperature resistant resin solution; step S2, placing the alumina aerogel in the high-temperature resistant resin solution, soaking it for a period of time, and then taking it out to obtain an alumina aerogel composite thermal insulation material precursor; and step S3, curing the alumina aerogel composite thermal insulation material precursor to obtain the alumina aerogel composite thermal insulation material.

[0016] Furthermore, the soaking time is 1 min to 5 h, preferably 1 to 3 h;

[0017] Preferably, the curing procedure is to cure at 180-260℃ for 1-4 hours, and then cure at 320-450℃ for 0.5-3 hours.

[0018] More preferably, the curing process is to cure at 180-230℃ for 2-4 hours, and then cure at 340-430℃ for 0.5-2 hours.

[0019] According to another aspect of this application, an alumina aerogel composite material is provided, which is prepared by the above-described alumina aerogel composite material raw material composition through the above-described preparation method; preferably, the content of the high-temperature resistant resin component in the alumina aerogel composite material is 0.01wt%-20wt%, more preferably 5wt%-20wt%.

[0020] By applying the technical solution of this invention, the high-temperature resistant resin not only significantly improves the compressibility of alumina aerogel, but also maintains its high-temperature resistance and thermal insulation properties. The high-temperature resistant alumina aerogel composite thermal insulation material prepared by this raw material composition has a service temperature resistance ≥1000℃. The above-mentioned alumina aerogel composite material raw material composition of this application can obtain a high-temperature resistant alumina aerogel composite thermal insulation material with high compressive strength through only two steps: impregnation and curing, which is convenient for application. Detailed Implementation

[0021] It should be noted that, unless otherwise specified, the embodiments and features described in this application can be combined with each other. The present invention will now be described in detail with reference to the embodiments.

[0022] As analyzed in the background section of this application, the existing technology has the problem of low compressive strength of alumina aerogel materials, which is prone to "flaking". In order to solve this problem, this application provides an alumina aerogel composite material raw material composition, an alumina aerogel composite material, and a method for preparing the same.

[0023] According to a typical embodiment of this application, an alumina aerogel composite material raw material composition is provided, the raw material composition comprising alumina aerogel and a high-temperature resistant resin raw material composition, wherein the high-temperature resistant resin raw material composition comprises a high-temperature resistant resin and an aprotic solvent.

[0024] The alumina aerogel composite material raw material composition of this application significantly improves the compressibility of alumina aerogel by using a high-temperature resistant resin, while maintaining the high-temperature resistance and thermal insulation properties of alumina aerogel. The high-temperature resistant alumina aerogel composite thermal insulation material prepared by this raw material composition has a service temperature resistance of ≥1000℃. The above-mentioned alumina aerogel composite material raw material composition of this application can obtain a high-temperature resistant alumina aerogel composite thermal insulation material with high compressive strength through only two steps: impregnation and curing, which is convenient for application.

[0025] In the high-temperature resistant resin raw material, other additives can also be selected from the prior art. This application does not limit this. In some typical embodiments of this application, the high-temperature resistant resin raw material includes high-temperature resistant resin, aluminum silver powder, aprotic solvent, anti-settling agent, coupling agent, and dispersant. Preferably, by weight, the high-temperature resistant resin raw material includes 10-50 parts of high-temperature resistant resin, 6-16 parts of aluminum silver powder, 30-85 parts of aprotic solvent, 1-7 parts of anti-settling agent, 0.01-5 parts of coupling agent, and 0.01-5 parts of dispersant. This can better leverage the synergistic effect of each component and further improve the compressive strength and thermal insulation performance of the alumina aerogel composite material. Among them, aluminum silver powder can improve the reflectivity of the coating, reduce the absorption of heat by the coating, and play a protective role. On the other hand, aluminum silver powder will form oxides during use, which have a certain thermal insulation effect.

[0026] The aforementioned high-temperature resistant resins can be selected from existing technologies, as long as they can withstand high temperatures (e.g., above 800°C) after curing. In some embodiments of this application, the aforementioned high-temperature resistant resins include any one or more of KB-8812, KB-8124, KB-8813, and KB-8124S, which are effective in improving the compressive strength and thermal insulation properties of the materials. In particular, KB-8812, when applied to the composite materials of this application, has a particularly significant effect on improving the aforementioned properties. The structural formula of KB-8812 resin is shown in Formula I:

[0027]

[0028] In Formula I, the ratio of m / n is 0.2 to 5.

[0029] The viscosity of KB-8812 resin is 50 to 3000 mPa·s, preferably 100 to 500 mPa·s.

[0030] The alumina aerogels described above can be selected from existing technologies. There are no particular requirements for the specific preparation method of the aerogel. In some embodiments of this application, the alumina aerogel includes alumina fibers. Preferably, the average diameter of the alumina fibers is 1-30 μm, more preferably 3-20 μm, resulting in a composite material with better overall performance. In some preferred embodiments of this application, the density of the alumina aerogel is 0.05-1 g / cm³. 3 Preferably, it is 0.1-0.6 g / cm³. 3 It has good thermal insulation performance.

[0031] The aforementioned aprotic solvents, antisettling agents, coupling agents, and dispersants can be selected from existing technologies, and other additives can be added according to the usage environment or actual needs. There are no special restrictions on the high-temperature resistant resin raw material in this regard.

[0032] In some embodiments of this application, the aforementioned aprotic solvent includes any one or more selected from dimethylformamide, dimethylacetamide, dimethyl sulfoxide, and n-butyl acetate. Exemplarily, the anti-settling agent includes any one or more selected from 201 anti-settling agent, fumed SiO2, high-clay, and talc, effectively preventing coating delamination. Exemplarily, the coupling agent includes any one or more selected from KH-560, KH-550, and KH-570. Dispersants may include any one or more selected from 232S dispersant, BYK-9076, BYK-171, BYK-174, and BYK-112.

[0033] In some typical embodiments of this application, the above-mentioned high-temperature resistant resin raw materials include 6-16 parts by weight of aluminum silver powder, 30-85 parts by weight of aprotic solvent, 1-7 parts by weight of 201 anti-settling agent, 10-50 parts by weight of KB-8812, 0.01-5 parts by weight of KH-560 coupling agent, and 0.01-5 parts by weight of 232S dispersant.

[0034] According to another typical embodiment of this application, a method for preparing an alumina aerogel composite material is provided. The preparation method includes: step S1, mixing any of the above-mentioned high-temperature resistant resin raw materials and stirring evenly to obtain a high-temperature resistant resin solution; step S2, placing the alumina aerogel in the high-temperature resistant resin solution, soaking it for a period of time, and then taking it out to obtain an alumina aerogel composite thermal insulation material precursor; step S3, curing the alumina aerogel composite thermal insulation material precursor to obtain the alumina aerogel composite thermal insulation material.

[0035] This application utilizes the aforementioned alumina aerogel composite material composition. By using a high-temperature resistant resin, it not only significantly improves the compressibility of alumina aerogel but also maintains its high-temperature resistance and thermal insulation properties. The high-temperature resistant alumina aerogel composite thermal insulation material prepared using this material composition has a service temperature resistance ≥1000℃. The above preparation method only requires two steps: impregnation and curing to obtain a high-temperature resistant alumina aerogel composite thermal insulation material with high compressive strength. The steps are simple and easy to operate.

[0036] In some embodiments of this application, the soaking time in step S2 is 1 min to 5 h, preferably 1 to 3 h. In some embodiments of this application, the curing procedure in step S3 is curing at 180-260°C for 1 to 4 h, followed by curing at 320-450°C for 0.5 to 3 h; preferably, the curing procedure is curing at 180-230°C for 2 to 4 h, followed by curing at 340-430°C for 0.5 to 2 h, resulting in alumina aerogel composite material with higher thermal insulation performance and compressive strength.

[0037] According to another typical embodiment of this application, an alumina aerogel composite material is provided, which is prepared from any of the above-described alumina aerogel composite material raw material compositions by any of the above-described preparation methods.

[0038] The aforementioned alumina aerogel composite material, through the use of a high-temperature resistant resin, not only significantly improves the compressibility of alumina aerogel but also maintains its high-temperature resistance. Furthermore, it exhibits low thermal conductivity, excellent thermal insulation performance, and chemical stability, making it a promising candidate for applications in the field of high-temperature insulation materials. Moreover, it can be prepared in just two steps: impregnation and curing, making the process simple and easy to operate.

[0039] In some embodiments of this application, the content of the high-temperature resistant resin component in the above-mentioned alumina aerogel composite material is 0.01wt%-20wt%, preferably 5wt%-20wt%; wherein the high-temperature resistant resin component is the above-mentioned high-temperature resistant resin raw material component, and the content of the high-temperature resistant resin component in the alumina aerogel composite material can be controlled by the viscosity of the high-temperature resistant resin raw material component and the impregnation time.

[0040] The beneficial effects that this application can achieve will be further illustrated below with reference to embodiments and comparative examples.

[0041] Example 1

[0042] First, prepare a high-temperature resistant resin solution, which contains: 6g aluminum silver powder, 85g dimethylformamide, 3g 201 anti-settling agent, 30g KB-8812 (viscosity 200mPa·s), 1g KH-560, and 0.5g 232S dispersant. Stir well.

[0043] With a density of 0.2 g / cm³ 3 The alumina aerogel felt was completely immersed in it for 2 hours, then removed and cured. The curing procedure was 3: cure at 180℃ for 3 hours, then raise the temperature to 390℃ and cure for 2 hours, then let it cool naturally to room temperature before removing it.

[0044] Based on weighing and calculation, the content of high-temperature resistant resin in the alumina aerogel composite insulation material of this embodiment is 8 wt%. The compressive strength of the alumina aerogel felt raw material is approximately 0.13 MPa, while the compressive strength of the high-temperature resistant alumina aerogel insulation material prepared in this embodiment is 3.4 MPa, an increase of 25 times. The thermal conductivity of the alumina aerogel raw material at room temperature is 0.022 W / (m·K), while the thermal conductivity of the high-temperature resistant alumina aerogel insulation material prepared in this embodiment is 0.023 W / (m·K). The addition of high-temperature resistant resin has almost no effect on thermal conductivity, resulting in excellent insulation performance. The results are summarized in Table 1.

[0045] Example 2

[0046] First, prepare a high-temperature resistant resin solution: aluminum silver powder: 5g, n-butyl acetate: 60g, 201 anti-settling agent: 5g, KB-8812 (viscosity 200mPa·s): 40g, KH-560: 0.5g, 232S dispersant: 1g, and stir evenly.

[0047] With a density of 0.2 g / cm³ 3 The alumina aerogel felt was completely immersed in it for 2 hours, then removed and cured. The curing procedure was as follows: cure at 220℃ for 1.5 hours, raise the temperature to 430℃ and cure for 0.5 hours, then let it cool naturally to room temperature before removing it.

[0048] Based on weighing and calculation, the content of high-temperature resistant resin in the alumina aerogel composite insulation material of this embodiment is 15 wt%. The compressive strength of the alumina aerogel raw material is approximately 0.13 MPa, while the compressive strength of the high-temperature resistant alumina aerogel insulation material prepared in this embodiment is 5.6 MPa, an increase of 42 times. The thermal conductivity of the alumina aerogel raw material at room temperature is 0.022 W / (m·K), while the thermal conductivity of the high-temperature resistant alumina aerogel insulation material prepared in this embodiment is 0.025 W / (m·K). The addition of the high-temperature resistant resin has almost no effect on the thermal conductivity, resulting in excellent insulation performance. The results are summarized in Table 1.

[0049] Example 3

[0050] The difference from Example 2 is that KB-8812 was replaced with the same weight of KB-8813 (viscosity 1500 mPa·s).

[0051] Example 4

[0052] The difference from Example 2 is that the amount of n-butyl acetate added is 30g.

[0053] Example 5

[0054] The difference from Example 2 is that the curing process is to cure at 390°C for 5 hours.

[0055] Example 6

[0056] The difference from Example 2 is that the curing procedure is as follows: cure at 280°C for 1.5 hours, then raise the temperature to 500°C and cure for 0.5 hours.

[0057] Example 7

[0058] The difference from Example 2 is that the soaking time is 30 minutes.

[0059] Example 8

[0060] The difference from Example 2 is that the soaking time is 5 hours.

[0061] The high-temperature resistant resin content, thermal conductivity, and compressive strength of the alumina aerogel raw materials and the alumina aerogel composite materials prepared in each embodiment are statistically analyzed in Table 1.

[0062] Table 1

[0063]

[0064] As can be seen from the above description, the above embodiments of the present invention achieve the following technical effects: the above-mentioned alumina aerogel composite material raw material composition, by using a high-temperature resistant resin, not only significantly improves the compressibility of alumina aerogel, but also maintains the high-temperature resistance and thermal insulation properties of alumina aerogel. The high-temperature resistant alumina aerogel composite thermal insulation material prepared by this raw material composition has a service temperature resistance ≥1000℃. The above-mentioned alumina aerogel composite material raw material composition of this application can obtain a high-temperature resistant alumina aerogel composite thermal insulation material with high compressive strength through only two steps: impregnation and curing, which is convenient for application.

[0065] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. 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 preparing an alumina aerogel composite material, characterized in that, include: Step S1: Mix the high-temperature resistant resin raw materials and stir evenly to obtain a high-temperature resistant resin solution; Step S2: Place the alumina aerogel in the high-temperature resistant resin solution, soak it for a period of time, and then take it out to obtain the alumina aerogel composite thermal insulation material precursor. Step S3: The alumina aerogel composite thermal insulation material precursor is cured to obtain the alumina aerogel composite thermal insulation material. The high-temperature resistant resin raw material includes high-temperature resistant resin and aprotic solvent; The content of the high-temperature resistant resin component in the alumina aerogel composite material is 5wt% - 20wt%. The aprotic solvent is selected from dimethylformamide and / or n-butyl acetate; The high-temperature resistant resin is selected from KB-8812.

2. The preparation method according to claim 1, characterized in that, The high-temperature resistant resin raw materials include high-temperature resistant resin, aluminum silver powder, aprotic solvent, anti-settling agent, coupling agent and dispersant.

3. The preparation method according to claim 1, characterized in that, By weight, the high-temperature resistant resin raw material includes 10-50 parts of high-temperature resistant resin, 6-16 parts of aluminum silver powder, 30-85 parts of aprotic solvent, 1-7 parts of anti-settling agent, 0.01-5 parts of coupling agent and 0.01-5 parts of dispersant.

4. The preparation method according to any one of claims 1 to 3, characterized in that, The alumina aerogel includes alumina fibers with an average diameter of 1-30 μm.

5. The preparation method according to claim 4, characterized in that, The alumina fibers have an average diameter of 3-20 μm.

6. The preparation method according to claim 4, characterized in that, The density of the alumina aerogel is 0.05-1 g / cm³. 3 .

7. The preparation method according to claim 4, characterized in that, The density of the alumina aerogel is 0.1-0.6 g / cm³. 3 .

8. The preparation method according to claim 2 or 3, characterized in that, The anti-settling agent includes any one or more selected from 201 anti-settling agent, fumed SiO2, high clay and talc.

9. The preparation method according to claim 2 or 3, characterized in that, The coupling agent includes any one or more selected from KH-560, KH-550 and KH-570; And / or, the dispersant includes any one or more selected from 232S dispersant, BYK-9076, BYK-171, BYK-174 and BYK-112.

10. The preparation method according to claim 1, characterized in that, The soaking time is 1 minute to 5 hours.

11. The preparation method according to claim 1, characterized in that, The soaking time is 1-3 hours.

12. The preparation method according to claim 1, characterized in that, The curing process involves curing at 180-260℃ for 1-4 hours, followed by curing at 320-450℃ for 0.5-3 hours.

13. The preparation method according to claim 1, characterized in that, The curing process involves curing at 180-230℃ for 2-4 hours, followed by curing at 340-430℃ for 0.5-2 hours.

14. An alumina aerogel composite material, characterized in that... It is prepared by the preparation method according to any one of claims 1 to 13.

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