Aerogel heat insulation felt and preparation method thereof

Abstract

The invention relates to a glass fiber aerogel heat insulation felt and a preparation method thereof. The heat insulation felt is prepared by the following steps: preparing composite slurry from raw materials including modified silicon dioxide aerogel, inorganic silicate modified resin, chopped glass fibers and the like according to a specific weight percentage, covering a glass fiber felt with the composite slurry, and sintering. Wherein the double coupling agent enables the chopped glass fibers and the aerogel to form an interwoven network structure, so that the interface bonding force is enhanced; the modified silicon dioxide aerogel reduces the water absorption rate and improves the structural compactness. The mechanical property of the obtained heat insulation felt is optimized, and the tear resistance is improved; the structural stability is enhanced, and the powder falling rate is remarkably reduced; the waterproof performance is excellent, a three-dimensional protection structure is formed, and technical guarantee is provided for application in a complex environment.

Description

Technical Field

[0001] This application relates to the field of thermal insulation materials technology, and in particular to an aerogel thermal insulation felt and its preparation method. Background Technology

[0002] Fiberglass aerogel insulation felt, as a functional material combining nanoporous structure and low thermal conductivity, has shown significant application value in building energy conservation and insulation, and industrial equipment insulation. However, current technology still faces key bottlenecks in material performance optimization and manufacturing process control, resulting in its overall performance failing to meet the requirements of complex working conditions, particularly in terms of mechanical strength, structural stability, and waterproof performance.

[0003] Existing glass fiber aerogel insulation felts generally suffer from insufficient mechanical properties due to weak interfacial bonding. Traditional processes use a single silane coupling agent to treat the glass fiber surface, achieving only limited bonding between the fiber and the resin matrix. The aerogel particles and fiber interface suffer from insufficient matching of acidic functional groups, resulting in weak interfacial shear strength and generally low overall compressive strength. This defect directly leads to delamination during transportation vibrations, cracking along the fiber interface during bending during construction, and even structural failure in scenarios requiring conformal deformation, such as pipe insulation. Furthermore, the uneven dispersion of chopped glass fibers further exacerbates the strength deficiency. Insufficient mechanical strength also directly leads to frequent dust shedding. Due to the weak bond between aerogel particles and the resin matrix, vibrations or airflow impacts during handling, installation, or long-term use easily cause aerogel particles to detach. This not only pollutes the construction environment and endangers the health of operators but also causes the effective thickness of the insulation felt to gradually decrease, destroying the nanoporous structure and ultimately leading to a gradual increase in thermal conductivity and a significant reduction in insulation performance.

[0004] In terms of waterproofing performance, existing processing techniques also have significant shortcomings. While a single surface spraying of a silane solution can form a hydrophobic film, the film has poor toughness and is prone to cracking under mechanical stress. More importantly, moisture can easily seep into the interior through microcracks at the fiber-aerogel interface, causing the aerogel to absorb water, swell, and collapse, further weakening the material's strength.

[0005] In summary, existing glass fiber aerogel insulation felts have systemic defects in terms of interfacial bonding strength, fiber dispersion, pore sealing effect, and waterproofing process. It is urgent to solve key problems such as insufficient mechanical properties, high powder shedding rate, and poor waterproofing durability through material formulation optimization and preparation process innovation, so as to promote the engineering application of this material. Summary of the Invention

[0006] This invention provides a composite slurry to solve the above-mentioned technical problems.

[0007] To solve the above-mentioned technical problems, the present invention provides a composite slurry, the composite slurry comprising: Modified silica aerogel 18%~22%; Inorganic silicate modified resin 32%~38%; 3%~5% chopped glass fiber; Dual coupling agent 0.3%~0.5%; Nano-clay dispersion 0.3%~0.5%; Defoamer 0.1%~0.3%; Wetting agent 0.2%~0.6%; 0.5% to 1.0% of methyltrimethoxysilane and / or vinyltrimethoxysilane; The remainder is water.

[0008] Furthermore, the dual coupling agent is a mixture of silane coupling agent and titanate coupling agent in a weight percentage ratio of (1~3):1.

[0009] The addition of chopped glass fibers and dual coupling agents synergistically enhances interfacial bonding. Silane coupling of chopped glass fibers and titanate coupling of aerogel improves interfacial shear strength and compressive strength, addressing the issue of insufficient mechanical strength. The interwoven network structure enhances the overall material integrity, improves tear resistance, and reduces the risk of breakage. Adding 0.5%-1.0% methyltrimethoxysilane and / or vinyltrimethoxysilane to the slurry allows it to penetrate internally and form silicon-oxygen-silicon bonds. The internal hydrophobic framework prevents moisture from penetrating into the aerogel pores at the source.

[0010] Furthermore, the dual coupling agent is a mixture of γ-aminopropyltriethoxysilane and pyrophosphate-type monoalkoxy titanate in a weight ratio of 2:1.

[0011] Furthermore, the modified silica aerogel was prepared using β-CD, silane coupling agent, silica sol, aminoadamantane, and halloysite nanotubes.

[0012] Furthermore, the mass ratio of the aminoadamantane, the silane coupling agent, and the silica sol is 1:1:(20~30); the mass ratio of the β-CD and the halloysite nanotubes is 1:(20~30).

[0013] Furthermore, the inorganic silicate modified resin is sodium silicate modified phenolic resin.

[0014] By modifying the resin with inorganic silicate to enhance the chemical cross-linking between the resin and the aerogel, the interfacial bonding strength is improved, interlayer delamination is reduced, the material toughness is improved, and the risk of fracture due to brittleness is reduced.

[0015] Furthermore, the method for preparing the modified silica aerogel includes the following steps: (1) Aminoadamantine and silane coupling agent are premixed evenly in proportion; aminoadamantine and silane coupling agent premixed solution is added to silica sol and stirred to form an "aminoadamantine-silica sol" complex. (2) Prepare a saturated aqueous solution of β-CD, and mix the β-CD solution with halloysite nanotubes to form a "β-CD-HNTs" complex; (3) Mix the “aminoadamantane-silica sol” complex from step (1) with the “β-CD-HNTs” complex from step (2) and stir to form a wet gel; The wet gel was dried to form a modified silica aerogel.

[0016] The modified silica aerogel preparation method utilizes the host-guest inclusion interaction of β-CD and aminoadamantane to construct a dynamic and reversible cross-linked network within the aerogel. The cyclic cavities of β-CD and aminoadamantane molecules form a "molecular switch" structure through non-covalent bonds. Under stress, the network dynamically dissociates to absorb energy, and rebonds after the external force disappears, endowing the material with self-healing capabilities. Halloysite nanotubes, after being coated with β-CD, cross-link with aminoadamantane-modified particles in the silica sol through hydrogen bonds, forming a multi-level anchoring structure of "glass fiber-β-CD-HNTs-aminoadamantane-silica sol," enhancing the interfacial bonding strength.

[0017] Furthermore, the preparation method of the composite slurry includes the following steps: (1) Raw materials are prepared according to weight percentage; (2) Mix water, inorganic silicate modified resin and modified silica aerogel, disperse and mix well to form a uniform base material; (3) Add the short glass fiber and nano clay dispersion, first shear and disperse, then add the double coupling agent and stir to mix well; (4) Add methyltrimethoxysilane, defoamer and wetting agent to adjust the viscosity of the slurry to 25~30mPa・s and pH value to 9~9.5 to obtain composite slurry.

[0018] The method for preparing the composite slurry employs high-shear dispersion to ensure uniform fiber dispersion; the addition of a coupling agent ensures sufficient interfacial reaction and improves bonding.

[0019] The present invention also provides an aerogel thermal insulation felt, which is prepared by sintering the above-mentioned composite slurry onto a fiber felt.

[0020] The present invention also provides a method for preparing the above-mentioned aerogel thermal insulation felt, the method comprising the following steps: (1) Pre-impregnate the fiber felt; (2) The pre-impregnated fiber felt is placed in an environment with a vacuum degree of -0.08MPa to -0.1MPa and impregnated with the composite slurry so that the slurry penetrates into the pores of the fiber felt; then, by extrusion, the amount of slurry coating on the surface of the fiber felt is controlled to be 1000~1200g / m²·mm.

[0021] (3) Sinter the impregnated fiber felt; (4) Surface hydrophobic treatment; (5) Drying is required.

[0022] The preparation method of the aerogel thermal insulation felt ensures that the composite slurry fills the pores of the fiber felt through impregnation, and the surface adsorption amount is precisely controlled to avoid local accumulation; gradient sintering eliminates micron-level pores, increases density, and simultaneously optimizes compressive strength and thermal insulation performance.

[0023] Furthermore, in step (4), the surface hydrophobic treatment uses a 5% volume concentration of SILRES® BS4004 solution as a hydrophobic agent. This can form a highly tough hydrophobic film to cover the surface microcracks, preventing external moisture from penetrating, while also enhancing surface abrasion resistance and further reducing the risk of powder shedding.

[0024] Furthermore, the fiber felt is selected from one of glass fiber felt, carbon fiber felt, nickel fiber felt, stainless steel fiber felt, aluminum silicate fiber felt, ceramic fiber felt, alumina fiber felt, basalt fiber felt, and polyacrylonitrile fiber felt.

[0025] Fiberglass mat is flexible and suitable for applications requiring bending, shaping, or as a reinforcing layer, such as thermal insulation, sound insulation, composite material reinforcement, filtration, environmental protection, and building decoration. It is particularly outstanding in fields requiring corrosion resistance, impact resistance, and lightweight properties.

[0026] Ceramic fiber felt is suitable for extreme environments with high temperature, high pressure, corrosion resistance, fire resistance and heat insulation due to its good rigidity and high temperature resistance. It is used in industrial kilns, aerospace, high temperature equipment sealing, protective equipment, energy-saving materials, etc., and performs particularly well in scenarios that need to withstand high temperature, mechanical vibration and chemical corrosion.

[0027] Fiberglass mat and ceramic fiber mat complement each other, covering a wide range of needs from everyday construction to cutting-edge technology.

[0028] Furthermore, the thickness of the fiber felt is 0.5-500 mm.

[0029] Furthermore, the coating amount of the composite slurry on the surface of the fiber felt is 0.5-50 kg / m². 2 .

[0030] As one embodiment of this application, the raw materials for preparing the modified silica aerogel include: Halloysite nanotubes; Dodecyl methacrylate and / or pentafluorophenyl methacrylate; Silica sol (SiO2 content 25%).

[0031] Furthermore, the raw materials for preparing the modified silica aerogel also include lightweight microspheres.

[0032] Furthermore, the lightweight microspheres include one or more of hollow glass microspheres, hollow silica microspheres, hollow ceramic microspheres, and phenolic resin hollow microspheres.

[0033] Furthermore, the particle size of the lightweight microspheres is 100-350 μm.

[0034] Furthermore, the density of the lightweight microspheres is 0.1-0.4 g / cm³. 3 .

[0035] Furthermore, the modified silica aerogel is prepared by copolymerizing halloysite nanotubes and silica sol.

[0036] Furthermore, the copolymer-modified halloysite nanotubes in the modified silica aerogel are connected to the silica sol via Si-O-Si bonds.

[0037] Furthermore, the surface of the copolymer-modified halloysite nanotubes is coated with pentafluorophenyl ester groups and dodecyl ester groups.

[0038] Furthermore, the copolymer-modified halloysite nanotubes are modified with dodecyl methacrylate and pentafluorophenyl methacrylate.

[0039] Furthermore, the preparation method of the copolymer-modified halloysite nanotubes includes the following steps: adding dodecyl methacrylate and / or pentafluorophenyl methacrylate, organic solvent and halloysite nanotubes into a reaction vessel, adding an initiator, controlling the reaction temperature at 70-80℃, stirring while reacting, reacting for 4-8 hours, cooling, filtering to collect the filter residue, washing, drying, and obtaining copolymer-modified halloysite nanotubes.

[0040] Furthermore, the halloysite nanotubes are coupling-modified halloysite nanotubes.

[0041] Furthermore, the preparation process of the coupling-modified halloysite nanotubes includes the following steps: adding silane coupling agent, water and pretreated halloysite nanotubes into a reaction vessel, adjusting the pH to 9-10, reacting at 60-80℃ for 2-3 hours, adjusting the pH to neutral, cooling, filtering, washing the filter residue, drying, and obtaining the copolymer-modified halloysite nanotubes.

[0042] Furthermore, the weight ratio of the silane coupling agent, water, and pretreated halloysite nanotubes is 1-1.5:100:9-14.

[0043] Furthermore, the preparation process of the pretreated halloysite nanotubes includes the following steps: mixing halloysite nanotubes with a weight ratio of (1:8-10) with a 20wt% urea solution, sonicating, allowing to stand, then adding a 5wt% sulfuric acid solution, allowing to stand, filtering, and drying to obtain the pretreated halloysite nanotubes; wherein, the weight ratio of sulfuric acid solution to halloysite nanotubes is 5:1.

[0044] The present invention also provides a method for preparing the above-mentioned composite slurry, comprising the following steps: (1) Raw materials are prepared according to weight percentage; (2) Mix water, inorganic silicate modified resin and modified silica aerogel, disperse and mix well to form a uniform base material; (3) Add the short glass fiber and nano clay dispersion, first shear and disperse, then add the double coupling agent and stir to mix well; (4) Add methyltrimethoxysilane, defoamer and wetting agent to adjust the viscosity of the slurry to 25~30mPa・s and pH value to 9~9.5 to obtain composite slurry.

[0045] To solve the above-mentioned technical problems, the present invention also provides an aerogel thermal insulation felt, wherein the aerogel thermal insulation felt is prepared by sintering a composite slurry as described in any one of claims 15-28 onto a fiber felt.

[0046] Furthermore, the preparation method of the aerogel insulation felt includes the following steps: (1) Pre-impregnate the fiber felt; (2) The pre-impregnated fiber felt is placed in an environment with a vacuum degree of -0.08MPa to -0.1MPa and impregnated with the composite slurry so that the composite slurry penetrates into the pores of the fiber felt; then, by extrusion, the amount of slurry coating on the surface of the fiber felt is controlled to be 1000~1200g / m²·mm.

[0047] (3) Sinter the impregnated fiber felt; (4) Surface hydrophobic treatment; (5) Drying is required.

[0048] Furthermore, in step (4), the surface hydrophobic treatment uses a 5% volume concentration of SILRES®BS4004 solution as a hydrophobic agent.

[0049] Furthermore, the fiber mat is selected from one of glass fiber mat, carbon fiber mat, nickel fiber mat, stainless steel fiber mat, aluminosilicate fiber mat, ceramic fiber mat, alumina fiber mat, basalt fiber mat, and polyacrylonitrile fiber mat. It can be used according to... Furthermore, the thickness of the fiber felt is 0.5-500 mm.

[0050] Furthermore, the coating amount of the composite slurry on the surface of the fiber felt is 0.5-50 kg / m². 2 .

[0051] Furthermore, the preparation method of the aerogel thermal insulation felt includes the following steps: coating the surface of the fiber felt with aerogel slurry, allowing it to stand until the fiber felt stably adsorbs the aerogel slurry, and drying it to obtain the aerogel thermal insulation felt.

[0052] Furthermore, the coating amount of the composite slurry on the surface of the fiber felt is 0.5-50 kg / m². 2 .

[0053] This application effectively improves the overall performance of fiberglass aerogel insulation felt through material formulation and process innovation: Mechanical property optimization: The use of a dual coupling agent system significantly enhances the interfacial bonding force between glass fiber and aerogel, improves the compressive strength and tear resistance of the material, and improves the problems of easy breakage and interlayer delamination in traditional processes.

[0054] By utilizing the host-guest inclusion relationship between β-CD and aminoadamantane, a dynamic and reversible cross-linked network is constructed within the aerogel. The cyclic cavities of β-CD and aminoadamantane molecules form a "molecular switch" structure through non-covalent bonds. Under stress, the network dynamically dissociates to absorb energy, and rebonds after the external force disappears, endowing the material with self-healing capabilities. After halloysite nanotubes are coated with β-CD, they cross-link with aminoadamantane-modified particles in the silica sol through hydrogen bonds, forming a multi-level anchoring structure of "glass fiber-β-CD-HNTs-aminoadamantane-silica sol," which enhances the interfacial bonding strength.

[0055] 3. Improved structural stability: By using high-filling nano-fillers and gradient pressure sintering process, aerogel pore defects are reduced, the risk of particle shedding is lowered, the powder shedding rate is significantly reduced, and the stability of thermal insulation performance is guaranteed.

[0056] 4. Breakthrough in waterproof performance: Adding 0.5%~1.0% methyltrimethoxysilane to the slurry allows it to penetrate the interior and form silicon-oxygen-silicon bonds. The internal hydrophobic skeleton prevents water from penetrating into the aerogel pores from the source. Combined with the surface hydrophobic membrane, it achieves "double protection inside and out" and reduces structural damage and powdering caused by water absorption.

[0057] 5. Dispersion and process adaptability: Innovative dispersion process and gradient temperature control optimize fiber dispersion uniformity, avoid adverse effects of high-temperature processes on material properties, and improve the stability and reliability of the preparation process.

[0058] The above improvements systematically solve existing technical bottlenecks through material interface control and process synergy optimization, providing technical support for the application of products in complex environments. Detailed Implementation

[0059] To describe the technical solutions of the above invention in more detail, specific embodiments are listed below to demonstrate the technical effects; it should be emphasized that these embodiments are used to illustrate the invention and not to limit the scope of the invention. To further illustrate the technical means and effects adopted by this application to achieve the intended purpose, the following detailed description, in conjunction with embodiments, provides a detailed explanation of the specific implementation methods, steps, features, and effects of the aerogel thermal insulation felt and its preparation method proposed in this application.

[0060] The foregoing and other technical contents, features and effects of this application can be more deeply and specifically understood through the description of specific embodiments, and are not intended to limit this application.

[0061] The sources of experimental materials in the embodiments and comparative examples of this application are as follows: β-CD: Cyclodextrin (β-CD for short), Qufu Tianli Pharmaceutical Excipients Co., Ltd. γ-aminopropyltriethoxysilane, abbreviated as KH-550, is manufactured by Nanjing Shuguang Chemical Group Co., Ltd. γ-Methacryloxypropyltrimethoxysilane, abbreviated as KH-570, Nanjing Shuguang Chemical Group Co., Ltd.; Aminoadamantane: Sichuan Zhongbang New Materials Co., Ltd.; Halloysite nanotubes (HNTs): Hefei Kejing Materials Technology Co., Ltd.; Silica sol: Zhejiang Yuda Chemical Co., Ltd. Short-cut glass fiber: Chongqing International Composite Materials Co., Ltd.; Titanate coupling agent TC-114: Nanjing Shuguang Chemical Group Co., Ltd.; Nano-montmorillonite dispersion (montmorillonite, solid content 20%): Zhejiang Fenghong New Material Co., Ltd. Methyltrimethoxysilane: Hubei Xinlantian New Materials Co., Ltd.; SILRES® BS4004 hydrophobic agent: Wacker Chemie (China) Co., Ltd.; Dodecyl methacrylate: Sigma-Aldrich, CAS No. 142-90-5.

[0062] Pentafluorophenyl methacrylate: TCI (Shanghai) Chemical Industry Development Co., Ltd., CAS No. 13642-97-2.

[0063] Inorganic silicate modified resin (phenolic modified sodium silicate resin): self-made Under the action of an acidic catalyst, the phenolic hydroxyl groups of phenolic resin and the silanic hydroxyl groups of sodium silicate undergo a condensation reaction to form Si-OC covalent bonds; the following raw materials are used in parts by weight: 80 parts sodium silicate, 25 parts methyl phenolic resin, 2 parts hydrochloric acid (catalyst, concentration 10%), and appropriate amount of water (to adjust viscosity); equipment: reaction vessel (with reflux condenser), high shear emulsifier, pH meter.

[0064] Operating steps: 1. Preparation of acidic sodium silicate: Sodium silicate was heated and stirred in a 60°C water bath, and ethanol was slowly added to dilute it to a solid content of 40%. The sodium silicate ethanol solution was then poured into a reaction vessel, and hydrochloric acid was slowly added dropwise while stirring to adjust the pH to 6.0~6.5. The sodium silicate was partially acidified to form nano-silica sol.

[0065] 2. Phenolic resin dispersion: Add methyl phenolic resin and disperse at a high shear rate of 1000 r / min for 15 minutes to form a uniform emulsion (phenolic resin particle size < 5 μm).

[0066] 3. Condensation reaction: The temperature was raised to 70℃ and the reaction was maintained for 3 hours. During this period, the hydroxymethyl (-CH2OH) and silanol (-SiOH) groups of the phenolic resin condensed, releasing water molecules, and the viscosity of the system gradually increased.

[0067] 4. Neutralization and filtration: The pH was adjusted to 8.5-9.0 (a weakly alkaline stable range) using sodium hydroxide solution, and the mixture was filtered to remove unreacted particles, thus obtaining phenolic modified sodium silicate resin.

[0068] Example 1 This example provides a glass fiber aerogel thermal insulation felt, and the preparation steps are as follows: Example 1.1 Preparation of modified silica aerogel: The following raw materials are used in parts by weight: The following mixture was prepared using 10 parts β-CD, 10 parts silane coupling agent KH-570, 250 parts silica sol (SiO2 content 25%), 10 parts aminoadamantane, and 250 parts halloysite nanotubes: Preparation process: (1) First, aminoadamantane and silane coupling agent KH-570 are premixed evenly to obtain a premixed solution; then, aminoadamantane and silane coupling agent KH-570 premixed solution are slowly added to silica sol, heated to 60°C, and stirred for 2 hours. Through the condensation of alkoxy groups (-OCH3) of silane coupling agent with hydroxyl groups (-SiOH) on the surface of silica sol, aminoadamantane molecules are grafted onto the surface of silica sol particles to form an "aminoadamantane-silica sol" complex. (2) Prepare a saturated aqueous solution of β-CD, add halloysite nanotubes to the β-CD aqueous solution, and disperse by ultrasonication at 30 kHz for 15 min to form a “β-CD-HNTs” complex; (3) Mix the “aminoadamantane-silica sol” complex obtained in step (1) with the “β-CD-HNTs” complex obtained in step (2) to form a wet gel by utilizing the host-guest inclusion effect of β-CD and aminoadamantane; (4) Modified silica aerogel is obtained after low-temperature drying.

[0069] Example 1.2 Preparation of composite slurry: Raw material composition, by weight percentage: 20% of the modified silica aerogel prepared in Example 1.1; 35% phenolic-modified sodium silicate resin; 4% chopped glass fiber (length 0.5~1mm, aspect ratio 8); 0.4% dual coupling agent (KH-550 to titanate coupling agent TC-114 weight ratio 2:1); Nano-montmorillonite dispersion 0.4%; Methyltrimethoxysilane 0.8%; Defoamer (TEGO® Foamex 844 and TEGO® Foamex 857, volume ratio 1:1) 0.2%; Wetting agents 0.3%: Disponer W-18 0.15% and Hydropalat® WE3221 0.15%; The remainder is water.

[0070] Preparation process: (1) Mix water, phenolic modified sodium silicate resin and modified silica aerogel, and disperse at 1600 r / min for 25 min to form a base material; (2) Add the short glass fiber and nano montmorillonite dispersion, first disperse at 1800 r / min for 18 min with high shear, then add the double coupling agent and stir for 12 min; (3) Finally, add methyltrimethoxysilane, defoamer and wetting agent to adjust the slurry viscosity to 28 mPa·s and the pH value to 9.2.

[0071] Example 1.3 Preparation of glass fiber aerogel insulation felt: Preparation process: (1) Pretreatment of glass fiber mat: The glass fiber mat was pre-soaked in a 3% silane coupling agent KH-550 solution for 20 min and then dried at 110℃ for 30 min.

[0072] (2) Vacuum impregnation: The pretreated fiber felt is placed in a vacuum environment of -0.08MPa and impregnated with the composite slurry prepared in Example 1.2 for 12min, so that the amount of composite slurry penetrating reaches 120% of the pore volume of the fiber felt. Then, the amount of slurry coated on the surface of the fiber felt is controlled to be 1000g / m² by roller extrusion. (3) The impregnated glass fiber mat is subjected to gradient pressure sintering at a heating rate of 8℃ / min, specifically: First stage: Hold at 180℃ and 0.5MPa pressure for 20 minutes to allow the resin to initially cure and fix the fiber position; Second stage: Maintain at 400℃ and 1.0MPa pressure for 20 min to promote chemical bonding between the coupling agent and the fiber / aerogel interface; The third stage: holding at 700℃ and 2.0MPa pressure for 20 minutes to increase the density to 0.38g / cm³ and eliminate micron-level pores; (4) Hydrophobic treatment Surface hydrophobic treatment: Prepare a 5% (v / v) hydrophobic solution with SILRES®BS4004 hydrophobic agent (a mixture of silane and siloxane) and soak for 30 minutes, then dry.

[0073] The glass fiber aerogel insulation felt obtained in this embodiment has significantly improved mechanical strength, reduced dust shedding, and waterproof performance.

[0074] Example 2: This example provides a glass fiber aerogel thermal insulation felt, and the preparation steps are as follows: Example 2.1 Preparation of modified silica aerogel: The following raw materials are used in parts by weight: The mixture was prepared by combining 10 parts of β-CD, 10 parts of silane coupling agent KH-570, 220 parts of silica sol (SiO2 content 25%), 10 parts of aminoadamantane, and 280 parts of halloysite nanotubes. The preparation method is the same as in Example 1. Example 2.2 Preparation of composite slurry: Raw material composition, by weight percentage: Modified silica aerogel 18%; Phenolic-modified sodium silicate resin 38%; 3% chopped glass fiber (length 0.5~1mm, aspect ratio 8); 0.5% dual coupling agent (KH-550 to titanate coupling agent TC-114 weight ratio 2:1); Nano-montmorillonite dispersion 0.3%; Methyltrimethoxysilane 0.8%; Defoamer (TEGO® Foamex 844 and TEGO® Foamex 857, volume ratio 1:1) 0.3%; Wetting agents 0.6%: Disponer W-18 0.3% and Hydropalat® WE3221 0.3%; The remainder is water.

[0075] Example 2.3 Preparation of glass fiber aerogel insulation felt: Glass fiber aerogel insulation felt was prepared using the composite slurry prepared in Example 2.2, and the preparation method was the same as in Example 1.3.

[0076] Example 3: This example provides a glass fiber aerogel thermal insulation felt, and the preparation steps are as follows: Example 3.1 Preparation of modified silica aerogel: The following raw materials are used in parts by weight: The mixture was prepared by combining 10 parts of β-CD, 10 parts of silane coupling agent KH-570, 280 parts of silica sol (SiO2 content 25%), 10 parts of aminoadamantane, and 220 parts of halloysite nanotubes. The preparation method is the same as in Example 1.

[0077] Example 3.2 Preparation of composite slurry: Raw material composition, by weight percentage: 22% modified silica aerogel; 32% phenolic-modified sodium silicate resin; 5% chopped glass fiber (length 0.5~1mm, aspect ratio 8); 0.3% dual coupling agent (KH-550 to titanate coupling agent TC-114 weight ratio 2:1); Nano-montmorillonite dispersion 0.3%; Methyltrimethoxysilane 0.6%; Defoamer (TEGO® Foamex 844 and TEGO® Foamex 857, volume ratio 1:1) 0.3%; Wetting agents 0.6%: Disponer W-18 0.3% and Hydropalat® WE3221 0.3%; The remainder is water.

[0078] Example 3.3 Preparation of glass fiber aerogel thermal insulation felt: Glass fiber aerogel insulation felt was prepared using the composite slurry prepared in Example 3.2, and the preparation method was the same as in Example 1.3.

[0079] Example 4: Example 4.1 Preparation of modified silica aerogel: Same as Example 1.1.

[0080] Example 4.2 Preparation of composite slurry: The preparation method of Example 5.2 is basically the same as that of Example 1.1. The difference is that in the preparation of the composite slurry in Example 4.2, 0.5% of a single coupling agent (KH-570) is used instead of 0.5% of the double coupling agent in Example 1.1 (KH-550 to titanate coupling agent TC-114 weight ratio 2:1).

[0081] Example 4.3 Preparation of glass fiber aerogel thermal insulation felt: Glass fiber aerogel insulation felt was prepared using the composite slurry prepared in Example 4.2, and the preparation method was the same as in Example 1.3.

[0082] Example 5: Example 5.1 Preparation of modified silica aerogel: Same as Example 1.1.

[0083] Example 5.2 Preparation of composite slurry: The preparation method of Example 5.2 is basically the same as that of Example 1.1. The difference is that in the preparation of glass fiber aerogel insulation felt in Example 5.2, methyltrimethoxysilane is not added to the composite slurry, while other raw materials, proportions, and steps are the same as in Example 1.2.

[0084] Example 5.3 Preparation of glass fiber aerogel thermal insulation felt: Glass fiber aerogel insulation felt was prepared using the composite slurry prepared in Example 5.2, and the preparation method was the same as in Example 1.3.

[0085] Example 6: Example 6.1 Preparation of modified silica aerogel: Percentage by weight The raw materials consist of 5% halloysite nanotubes, 3% dodecyl methacrylate, 2% pentafluorophenyl methacrylate, and the remainder being silica sol (SiO2 content 25%).

[0086] Preparation process: (1) Mix halloysite nanotubes with dodecyl methacrylate and pentafluorophenyl methacrylate, and ultrasonically disperse for 30 min to complete surface modification; (2) Modified nanotubes were added to silica sol and stirred evenly to gel. After aging, methanol solvent exchange and CO2 supercritical drying, modified silica aerogel was obtained.

[0087] The other components and preparation methods are the same as in Example 1.

[0088] Example 6.2 Preparation of composite slurry: Composite slurry was prepared using the modified silica aerogel prepared in Example 6.1. Other raw materials and preparation steps were the same as in Example 1.2.

[0089] Example 6.3 Preparation of glass fiber aerogel insulation felt: Glass fiber aerogel insulation felt was prepared using the composite slurry prepared in Example 6.2, and the preparation method was the same as in Example 1.3.

[0090] Example 7: Example 7.1 Preparation of modified silica aerogel: In the preparation of modified silica aerogels, inclusion with β-CD solution is not used: The following raw materials are used in parts by weight: The mixture was prepared by combining 10 parts of silane coupling agent KH-570, 250 parts of silica sol (SiO2 content 25%), 10 parts of aminoadamantane, and 250 parts of halloysite nanotubes.

[0091] Preparation process: (1) Aminodane and silane coupling agent KH-570 are premixed evenly to obtain a premixed solution; the premixed solution of aminodane and silane coupling agent KH-570 is slowly added to the silica sol, the temperature is raised to 60℃, and the mixture is kept warm and stirred for 2 hours. The alkoxy group (-OCH3) of the silane coupling agent is condensed with the hydroxyl group (-SiOH) on the surface of the silica sol to achieve the grafting of aminodane molecules onto the surface of the silica sol particles to form an "aminodane-silica sol" complex. (2) Add halloysite nanotubes to the “aminoadamantane-silica sol” composite obtained in step (1) and stir until homogeneous before gelling; (3) Modified silica aerogel is obtained after low-temperature drying.

[0092] Example 7.2 Preparation of composite slurry: Composite slurry was prepared using the modified silica aerogel prepared in Example 7.1, with other raw materials and preparation steps being the same as in Example 1.2.

[0093] Example 7.3 Preparation of glass fiber aerogel insulation felt: Glass fiber aerogel insulation felt was prepared using the composite slurry prepared in Example 7.2, and the preparation method was the same as in Example 1.3.

[0094] Example 8: Example 8.1 Preparation of modified silica aerogel: In the preparation of modified silica aerogel, aminoadamantane is not added: (1) Prepare a saturated aqueous solution of β-CD, add halloysite nanotubes to the β-CD aqueous solution, and disperse by ultrasonication at 30 kHz for 15 min to form a “β-CD-HNTs” complex; (2) Add silane coupling agent KH-570 to silica sol, heat to 60°C, stir for 2 hours, add the “β-CD-HNTs” complex obtained in step (1) and mix. After stirring evenly, gel. (3) Modified silica aerogel is obtained after low-temperature drying.

[0095] Example 8.2 Preparation of composite slurry: Composite slurry was prepared using the modified silica aerogel prepared in Example 8.1, with other raw materials and preparation steps being the same as in Example 1.2.

[0096] Example 8.3 Preparation of glass fiber aerogel insulation felt: Glass fiber aerogel insulation felt was prepared using the composite slurry prepared in Example 8.2, and the preparation method was the same as in Example 1.3. Example 9:

[0097] Example 9.1 Preparation of modified silica aerogel: In the preparation of modified silica aerogel, no silane coupling agent KH-570 is added: (1) Prepare a saturated aqueous solution of β-CD, add halloysite nanotubes to the β-CD aqueous solution, and disperse by ultrasonication at 30 kHz for 15 min to form a “β-CD-HNTs” complex; (2) Add aminoadamantine to silica sol, heat to 60°C, stir for 2 hours, add the “β-CD-HNTs” complex obtained in step (1) and mix, stir evenly and then gel. (3) Modified silica aerogel is obtained after low-temperature drying.

[0098] Example 9.2 Preparation of composite slurry: Composite slurry was prepared using the modified silica aerogel prepared in Example 9.1, with other raw materials and preparation steps being the same as in Example 1.2.

[0099] Example 9.3 Preparation of glass fiber aerogel insulation felt: Glass fiber aerogel insulation felt was prepared using the composite slurry prepared in Example 9.2, and the preparation method was the same as in Example 1.3. Example 10:

[0100] Example 10.1 Preparation of modified silica aerogel: Percentage by weight The raw materials consist of 5% halloysite nanotubes, 5% pentafluorophenyl methacrylate, and the remainder being silica sol (SiO2 content 25%).

[0101] Preparation process: (1) Mix halloysite nanotubes with pentafluorophenyl methacrylate and ultrasonically disperse for 30 min to complete surface modification; (2) Modified nanotubes were added to silica sol and stirred evenly to gel. After aging, methanol solvent exchange and CO2 supercritical drying, modified silica aerogel was obtained.

[0102] The other components and preparation methods are the same as in Example 1.

[0103] Example 10.2 Preparation of composite slurry: The composite slurry was prepared using the modified silica aerogel prepared in Example 10.1. The 0.8% methyltrimethoxysilane in Example 1.2 was replaced with 0.8% vinyltrimethoxysilane. Other raw materials and preparation steps were the same as in Example 1.2.

[0104] Example 10.3 Preparation of glass fiber aerogel thermal insulation felt: Glass fiber aerogel thermal insulation felt was prepared using the composite slurry prepared in Example 10.2, and the preparation method was the same as in Example 1.3.

[0105] Example 11: Example 11.1 Preparation of modified silica aerogel: Percentage by weight The raw materials consist of 5% halloysite nanotubes, 5% dodecyl methacrylate, and the remainder being silica sol (SiO2 content 25%).

[0106] Preparation process: (1) Mix halloysite nanotubes with dodecyl methacrylate and ultrasonically disperse for 30 min to complete surface modification; (2) Modified nanotubes were added to silica sol and stirred evenly to gel. After aging, methanol solvent exchange and CO2 supercritical drying, modified silica aerogel was obtained.

[0107] The other components and preparation methods are the same as in Example 1.

[0108] Example 11.2 Preparation of composite slurry: The composite slurry was prepared using the modified silica aerogel prepared in Example 11.1. The 0.8% methyltrimethoxysilane in Example 1.2 was replaced with: 0.4% methyltrimethoxysilane + 0.4% vinyltrimethoxysilane. Other raw materials and preparation steps were the same as in Example 1.2.

[0109] Example 11.3 Preparation of glass fiber aerogel insulation felt: Glass fiber aerogel insulation felt was prepared using the composite slurry prepared in Example 11.2, and the preparation method was the same as in Example 1.3.

[0110] Comparative Example 1: Comparative Example 1.1 Unmodified silica aerogel Ordinary unmodified silica aerogel was used instead of the modified silica aerogel in Example 1.1.

[0111] Comparative Example 1.2 Preparation of Composite Slurry: The modified silica aerogel prepared in Comparative Example 1.1 was used to prepare the composite slurry. Other raw materials and preparation steps were basically the same as in Example 1.2. The only difference was that in the preparation of the composite slurry, step (2) was kept at a high shear dispersion of 1800 r / min. Due to the decrease in the dispersibility of ordinary silica aerogel, the stirring time was extended to 30 min.

[0112] Comparative Example 1.3 Preparation of glass fiber aerogel insulation felt: Glass fiber aerogel insulation felt was prepared using the composite slurry prepared in Comparative Example 1.2, and the preparation method was the same as in Example 1.3.

[0113] test: I. 30-minute burn-through test of thermal insulation materials Test samples: Glass fiber aerogel thermal insulation felt prepared in Examples 1, 2, 3, 4 to Comparative Example 1; Test method: GB / T25352-2010; Test equipment: oil burner; Flame temperature (°C): 1022~1044; Fuel parameters: Flow rate: (6.0~6.2) gph; Pressure: (100~120) psi; Temperature: (0~11) ℃; Air parameters: Pressure: (63~67) psi; Temperature: (4~16) ℃; Sample pretreatment: Temperature: 21.9℃~22.8℃; Humidity: 51%~62%; Time: 25h.

[0114] Experimental data: Table 1: Burn-through test results of glass fiber aerogel insulation felt prepared in Examples 1, 2, 3, 4 to Comparative Example 1.

[0115] sample Whether it burned through and the time of occurrence (s) Maximum heat flux (W / cm²) and time of occurrence (s) on the back side Example 1 Not burned through Left:0.63 / 1790; Right:0.67 / 1793 Example 2 Not burned through Left:0.69 / 1788; Right:0.70 / 1796 Example 3 Not burned through Left:0.65 / 1798; Right:0.68 / 1800 Example 4 Not burned through Left:0.93 / 1772; Right:0.89 / 1789 Example 5 Not burned through Left:0.81 / 1785; Right:0.79 / 1796 Example 6 Not burned through Left:0.89 / 1745; Right:0.85 / 1777 Example 7 Not burned through Left:0.89 / 1788; Right:0.85 / 1786 Example 8 Not burned through Left:0.82 / 1760; Right:0.79 / 1780 Example 9 Not burned through Left:0.84 / 1760; Right:0.81 / 1780 Example 10 Not burned through Left:0.86 / 1757; Right:0.87 / 1779 Example 11 Not burned through Left:0.88 / 1747; Right:0.89 / 1791 Comparative Example 1 It did not burn through, but the edges were carbonized. Left: 1.35 / 1700; Right: 1.30 / 1720 As can be seen from the data in Table 1: the fiberglass aerogel insulation felts obtained in Examples 1-3 did not burn through within 30 minutes and their structures remained intact; although the insulation felts obtained in Examples 4-11 also did not burn through within 30 minutes, their heat flux values ​​were significantly higher than those obtained in Examples 1-3; the insulation felt obtained in Comparative Example 1 did not burn through but its edges were carbonized, and its heat flux value reached 1.30 W / cm². The reason for this is that the back heat flux values ​​in Examples 1-3 were all below 0.7 W / cm². The key factor is that the modified aerogel encapsulates aminoadamantane with β-cyclodextrin (β-CD) to form a dynamic cross-linked network, effectively blocking the heat conduction path. The dual coupling agent enhances the structural density.

[0116] Example 4 uses a single coupling agent, possibly because a single silane coupling agent cannot bond the modified silica aerogel, resulting in high interfacial thermal resistance and a significant increase in thermal conductivity, leading to a significantly higher heat flux value than in Examples 1-3.

[0117] Example 5 was not treated with hydrophobic material, and the internal pores were not hydrophobic. After absorbing water, the thermal conductivity of the aerogel increased, and the structural expansion led to an increase in pore defects, resulting in a higher heat flux value than in Examples 1-3.

[0118] Examples 6 and 7 lack β-CD inclusion and dynamic cross-linking network, which cannot suppress microcrack propagation at high temperatures. The heat conduction path increases, resulting in a significantly higher heat flux value than Examples 1-3.

[0119] Examples 8 and 9 may be due to uneven dispersion of aerogel particles, loose structure, and increased heat transfer due to air convection, resulting in higher heat flux values.

[0120] Comparative Example 11 uses ordinary silica aerogel. Ordinary aerogel has strong water absorption. At high temperature, water evaporates to form water vapor channels, which increases thermal conductivity.

[0121] This leads to the conclusion that the compactness of the structure constructed by the dual coupling agent and the construction of a dynamic reversible cross-linked network within the modified silica aerogel using the host-guest encapsulation effect of β-CD and aminoadamantane are key to improving the thermal insulation performance.

[0122] II. Mechanical Property Testing 1. Tensile Strength and Elongation at Break: Five specimens with dimensions of 100 mm × 20 mm were cut from the glass fiber aerogel insulation felt prepared in Examples 1, 2, 3, 4 to Comparative Example 1. Tensile tests were performed on the specimens using a universal testing machine at a tensile speed of 5 mm / min. The maximum tensile force and elongation at break were recorded, and the tensile strength (unit: MPa) and elongation at break (unit: %) were calculated.

[0123] 2. Bending Strength: Five 100mm × 20mm specimens were cut from the glass fiber aerogel insulation felts of Examples 1, 2, 3, 4 to Comparative Example 1. A three-point bending test was conducted on a universal testing machine with a span of 60mm and a loading speed of 1mm / min. The maximum load at which the specimen broke was recorded, and the bending strength (unit: MPa) was calculated.

[0124] 3. Test Results Table 2: Mechanical property test results of glass fiber aerogel insulation felt in Examples 1, 2, 3, 4 to Comparative Example 1.

[0125] sample Tensile strength (MPa) Elongation at break (%) Bending strength (MPa) Example 1 3.62±0.04 17.0±1.1 2.91±0.16 Example 2 3.51±0.06 16.5±1.0 2.75±0.15 Example 3 3.41±0.05 16.0±1.2 2.82±0.18 Example 4 2.98±0.07 13.0±0.9 2.40±0.18 Example 5 3.30±0.08 15.5±0.8 2.70±0.15 Example 6 2.96±0.08 13.5±0.8 2.35±0.15 Example 7 3.01±0.09 14.0±0.7 2.30±0.16 Example 8 2.78±0.08 13.8±0.6 2.35±0.17 Example 9 2.65±0.06 13.5±0.8 2.30±0.12 Example 10 2.60±0.08 12.5±0.6 2.20±0.14 Example 11 2.71±0.06 11.9±0.7 2.18±0.12 Comparative Example 1 2.20±0.05 11.0±0.5 2.10±0.10 As can be seen from the experimental data in Table 2: Comparative Example 1 uses commercially available ordinary silica aerogel. Compared with Comparative Example 1, the mechanical properties of Examples 1-11 are all improved, highlighting the revolutionary improvement of the aerogel interface performance by the modification process. Chemical modification can improve the interfacial bonding strength.

[0126] Analysis of the mechanical property test results shows that the mechanical properties of Examples 1-3 and Example 5 are significantly better than those of other examples. This indicates that the use of a dual coupling agent system and a β-CD-HNTs-aminoadamantane structure significantly enhances the interfacial bonding force between glass fiber and aerogel, imparts flexibility to the material, and improves the material's compressive strength, tensile strength, and tear resistance.

[0127] Example 4 uses a single coupling agent. Compared to Example 4, Examples 1-3 use dual coupling agents, and the mechanical properties of Examples 1-3 are higher than those of Example 4. This may be because a single silane coupling agent can only form Si-O bonds with hydroxyl groups (-OH) on the glass fiber surface through alkoxy groups (-OCH3), but cannot effectively react with acidic groups (such as silanol groups) on the aerogel surface, resulting in only a physical adsorption layer forming at the fiber-aerogel interface, with insufficient shear strength. The dual coupling agents in Examples 1-3 can synergistically enhance the interfacial bonding force, and the titanate coupling agent can increase the chemical crosslinking density between the aerogel and the resin, thereby optimizing the mechanical properties.

[0128] Example 5 did not contain methyltrimethoxysilane. Compared with Example 5, Examples 1-3 contained methyltrimethoxysilane. Therefore, the mechanical properties of Examples 1-3 were higher than those of Example 5.

[0129] The modified silica aerogel in Example 6 was prepared by methacrylate modification, replacing the β-CD inclusion process; compared with Example 6, Examples 1-3 used the β-CD inclusion process, so the mechanical properties of Examples 1-3 were significantly improved.

[0130] In Example 7, the β-CD solution inclusion process was omitted in the preparation of the modified silica aerogel; instead, aminoadamantane, silica sol, and halloysite nanotubes were directly mixed. Compared to Example 7, Examples 1-3 employed a β-CD inclusion process, thus significantly improving the mechanical properties of Examples 1-3. This is because... In Examples 1-3, the cyclic cavity encapsulation of aminoadamantane with β-CD resulted in the formation of "dynamic cross-linking nodes" within the aerogel. However, Example 7 lacked the cyclic cavity encapsulation of aminoadamantane with β-CD, and thus no "dynamic cross-linking nodes" formed within the aerogel. This resulted in stress concentration under stress, leading to rapid microcrack propagation. A comparison of the data from Examples 1-3 and Example 7 demonstrates that β-CD encapsulation is the core of constructing a multi-level anchoring structure, enhancing the interfacial synergistic deformation capability through host-guest interaction.

[0131] In Examples 8 and 9, no aminoadamantane or silane coupling agents were used in the preparation of the modified silica aerogels. Compared with Examples 8 and 9, Examples 1-3 used aminoadamantane or silane coupling agents, resulting in significantly improved mechanical properties. This is because aminoadamantane was grafted onto the silica sol surface in Examples 1-3, forming a host-guest inclusion complex with β-CD, resulting in a denser aerogel structure, fewer internal pore defects, and increased load-bearing capacity. In contrast, the mechanical properties of Examples 8 and 9 were worse than the examples, possibly because the silica sol surface was not grafted with aminoadamantane, preventing the formation of a host-guest inclusion complex with β-CD, leading to a looser aerogel structure, increased internal pore defects, and decreased load-bearing capacity. A comparison of the data from Examples 1-3 with those from Examples 8-9 shows that aminoadamantane grafting and silane coupling agent treatment have a dual effect on improving aerogel density and fiber interfacial adhesion.

[0132] In summary, Examples 1-3 demonstrate that the compactness of the structure constructed with dual coupling agents and the use of β-CD and aminoadamantane as host-guest inclusion agents to build a dynamic reversible cross-linked network within the aerogel are key to improving thermal insulation performance.

[0133] III. Anti-dust performance test 1. Test Samples: Glass fiber aerogel insulation felts from Examples 1, 2, 3, 4 to Comparative Example 1 were selected to ensure that the sample sizes were the same and that three copies of each sample were prepared for parallel testing to improve the accuracy and reliability of the test results.

[0134] 2. Test equipment: The dust shedding rate test device includes a sealed chamber, a vibration device, a dust collector, and an electronic balance.

[0135] 3. Experimental Procedure: (1) Weigh the initial mass of each sample using an electronic balance and record it accurately.

[0136] (3) Place the sample into the sealed box of the dust loss rate test device, set the vibration frequency to 50Hz and the vibration time to 60 minutes, and start the vibration device and dust collector to begin the test.

[0137] (3) After the test, weigh the collected dust using an electronic balance and record the data.

[0138] (4) Repeat the above steps for each sample, for a total of 3 tests.

[0139] 4. Data processing and calculation: According to the formula "Dust shedding rate (%) = (collected dust mass ÷ initial sample mass) × 100%", calculate the dust shedding rate for each test, and then take the average of the three test results for each sample as the dust shedding rate of that sample.

[0140] 5. Test Data Table 3. Test results of dust shedding performance of glass fiber aerogel thermal insulation felt in Examples 1, 2, 3, 4 to Comparative Example 1.

[0141] sample Initial sample mass (g) Dust mass (g) after the first vibration Dust mass (g) after the second vibration Dust mass (g) after the third vibration Average dust mass (g) Fan loss rate (%) Example 1 50.000 0.120 0.100 0.080 0.100 0.20 Example 2 50.000 0.140 0.120 0.100 0.120 0.24 Example 3 50.000 0.200 0.120 0.130 0.150 0.30 Example 4 50.000 0.300 0.250 0.200 0.250 0.50 Example 5 50.000 0.250 0.210 0.170 0.210 0.42 Example 6 50.000 0.500 0.400 0.300 0.400 0.80 Example 7 50.000 0.550 0.400 0.400 0.450 0.90 Example 8 50.000 0.400 0.350 0.300 0.350 0.70 Example 9 50.000 0.500 0.400 0.450 0.450 0.9 Example 10 50.000 0.550 0.450 0.350 0.450 0.90 Example 11 50.000 0.500 0.450 0.300 0.420 0.84 Comparative Example 1 50.000 0.800 0.650 0.500 0.650 1.30 As can be seen from the experimental data in Table 3: Comparative Example 1 uses commercially available ordinary silica aerogel. Compared with Comparative Example 1, the powder shedding rate of Examples 1-11 is significantly reduced, highlighting the disruptive improvement of aerogel interface performance by the modification process.

[0142] The dust shedding rate of the glass fiber aerogel insulation felt in Examples 1-3 was significantly lower than that in Examples 4-11 and Comparative Example 1. This indicates that the technical solutions adopted in Examples 1-3, such as the β-CD solution encapsulation modification of silica aerogel, the dual coupling agent system, and the internal hydrophobic treatment, can effectively reduce the dust shedding rate of the glass fiber aerogel insulation felt and improve the stability and reliability of the product.

[0143] Example 4 uses a single coupling agent. Compared to Example 4, Examples 1-3 use dual coupling agents, resulting in a lower powder shedding rate in Examples 1-3 compared to Example 4. Examples 1-3 use dual coupling agents; the "anchoring and bridging" effect of the titanate coupling agent strengthens the interparticle constraint, enabling bonding of glass fibers and forming an effective anchor with the aerogel particles. This results in a tight connection between the aerogel particles and the resin matrix, making them less prone to detachment during vibration. In contrast, Example 4 uses a single silane coupling agent, lacking the "anchoring and bridging" effect of the titanate coupling agent. This leads to insufficient interparticle constraint, only bonding to glass fibers and failing to form an effective anchor with the aerogel particles. This results in micron-level gaps between the aerogel particles and the resin matrix, making them prone to detachment during vibration. A comparison of the data from Examples 1-3 and Example 4 demonstrates the necessity of dual coupling agents synergistically enhancing interfacial adhesion. The titanate coupling agent can "weld" the aerogel particles to the fiber surface, reducing the risk of detachment.

[0144] Example 5 did not include methyltrimethoxysilane. Compared to Example 5, Examples 1-3 included methyltrimethoxysilane, and the powder shedding rate in Examples 1-3 was significantly lower than in Example 5. This is because the addition of methyltrimethoxysilane in Examples 1-3 can inhibit powder shedding caused by water absorption at the source. In contrast, the lack of hydrophobic treatment in Example 5 resulted in the aerogel's internal pores not being hydrophobicized. Water penetration triggered a swelling-shrinkage cycle in the aerogel particles, weakening interfacial adhesion. A comparison of the data from Examples 1-3 with that of Example 5 demonstrates the crucial role of the "internal hydrophobic framework" in structural stability, and that methyltrimethoxysilane can inhibit powder shedding caused by water absorption at the source.

[0145] In Example 6, the modified silica aerogel was prepared using methacrylate modification instead of the β-CD inclusion process. Compared to Example 6, Examples 1-3 used the β-CD inclusion process, and the powder loss rate of Examples 1-3 was significantly lower than that of Example 6. This is because the β-CD inclusion process used in Examples 1-3 resulted in a rigid cross-linked network formed by methacrylate modification, and the dynamic reversible inclusion effect between β-CD and aminoadamantane made it less prone to brittle fracture under stress. In contrast, Example 6, while also using methacrylate modification to form a rigid cross-linked network, lacked the dynamic reversible inclusion effect between β-CD and aminoadamantane, making it prone to brittle fracture under stress and releasing aerogel particles. The halloysite nanotubes were not coated with β-CD, their surface hydroxyl groups were not activated, and they were only physically entangled with the aerogel particles, making them prone to slippage under vibration.

[0146] In the preparation of modified silica aerogel in Example 7, β-CD solution inclusion was omitted, and aminoadamantane, silica sol and halloysite nanotubes were directly mixed. Compared with Example 7, Examples 1-3 used β-CD solution inclusion, and the powder loss rate of Examples 1-3 was significantly lower than that of Example 7. The comparison between the data of Examples 1-3 and the data of Example 7 shows that β-CD inclusion is the core of building a dense structure, which improves the interparticle binding energy and reduces the powder loss rate through host-guest interaction.

[0147] In Examples 8 and 9, no aminoadamantane or silane coupling agent was used in the preparation of the modified silica aerogel. Compared with Examples 8 and 9, Examples 1-3 used aminoadamantane or silane coupling agents, and the powder shedding rate of Examples 1-3 was significantly lower than that of Examples 8 and 9. In Examples 1-3, aminoadamantane was grafted onto the surface of the silica sol. The aminoadamantane grafting and silane coupling agent improved the interfacial bonding density, and the two synergistically formed a "multi-point anchoring" structure. In contrast, the silica sol surface in Examples 8 and 9 was not grafted with aminoadamantane, resulting in the aerogel particles being dispersed in an "island-like" pattern, reducing the interfacial bonding area. The lack of hydrophobic modification of the glass fiber by the silane coupling agent resulted in weak chemical bonding between the hydroxyl groups on the fiber surface and the aerogel, making the particles prone to sliding and falling off along the fiber axis. The effects of aminoadamantane grafting and silane coupling agent treatment on improving the interfacial bonding density are emphasized, and the two synergistically form a "multi-point anchoring" structure.

[0148] The above description is merely a preferred embodiment of the invention and is not intended to limit the scope of this application in any way. Although the preferred embodiment has been disclosed above, it is not intended to limit the application. Any person skilled in the art can make some modifications or alterations to the disclosed technical content to create equivalent embodiments without departing from the scope of the technical solution of this application. Any simple modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of this application without departing from the scope of the technical solution of this application shall still fall within the scope of the technical solution of this application.

[0149] The following raw materials are used in parts by weight: The following mixture was prepared using 10 parts β-CD, 10 parts silane coupling agent KH-570, 250 parts silica sol (SiO2 content 25%), 10 parts aminoadamantane, and 250 parts halloysite nanotubes: Preparation process: (1) First, aminoadamantane and silane coupling agent KH-570 are premixed evenly to obtain a premixed solution; then, aminoadamantane and silane coupling agent KH-570 premixed solution are slowly added to silica sol, heated to 60°C, and stirred for 2 hours. Through the condensation of alkoxy groups (-OCH3) of silane coupling agent with hydroxyl groups (-SiOH) on the surface of silica sol, aminoadamantane molecules are grafted onto the surface of silica sol particles to form an "aminoadamantane-silica sol" complex. (2) Prepare a saturated aqueous solution of β-CD, add halloysite nanotubes to the β-CD aqueous solution, and disperse by ultrasonication at 30 kHz for 15 min to form a “β-CD-HNTs” complex; (3) Mix the “aminoadamantane-silica sol” complex obtained in step (1) with the “β-CD-HNTs” complex obtained in step (2) to form a wet gel by utilizing the host-guest inclusion effect of β-CD and aminoadamantane; (4) Modified silica aerogel is obtained after low-temperature drying.

Claims

1. A composite slurry, characterized in that, The composite slurry includes: Modified silica aerogel 18%~22%; Inorganic silicate modified resin 32%~38%; 3%~5% chopped glass fiber; Dual coupling agent 0.3%~0.5%; Nano-clay dispersion 0.3%~0.5%; Defoamer 0.1%~0.3%; Wetting agent 0.2%~0.6%; 0.5% to 1.0% of methyltrimethoxysilane and / or vinyltrimethoxysilane; The remainder is water.

2. The composite slurry according to claim 1, characterized in that, The dual coupling agent is a mixture of silane coupling agent and titanate coupling agent in a weight percentage ratio of (1~3):

1.

3. The composite slurry according to claim 1, characterized in that, The dual coupling agent is a mixture of γ-aminopropyltriethoxysilane and pyrophosphate-type monoalkoxy titanate in a weight ratio of 2:

1.

4. The composite slurry according to any one of claims 1-3, characterized in that, The modified silica aerogel was prepared using β-CD, silane coupling agent, silica sol, aminoadamantane, and halloysite nanotubes.

5. The composite slurry according to claim 4, characterized in that, The mass ratio of the aminoadamantane, the silane coupling agent, and the silica sol is 1:1:(20~30); the mass ratio of the β-CD and the halloysite nanotubes (HNTs) is 1:(20~30).

6. The composite slurry according to any one of claims 1-5, characterized in that, The inorganic silicate modified resin is sodium silicate modified phenolic resin.

7. The composite slurry according to any one of claims 1-6, characterized in that, The method for preparing modified silica aerogel includes the following steps: (1) Aminoadamantine and silane coupling agent are premixed evenly in proportion; aminoadamantine and silane coupling agent premixed solution is added to silica sol and stirred to form an "aminoadamantine-silica sol" complex. (2) Prepare a saturated aqueous solution of β-CD, and mix the β-CD solution with HNTs to form a "β-CD-HNTs" complex; (3) Mix the "aminoadamantane-silica sol" complex from step (1) with the "β-CD-HNTs" complex from step (2) and stir to form a wet gel; The wet gel was dried to form a modified silica aerogel.

8. The composite slurry according to any one of claims 1-7, characterized in that, The preparation method of the composite slurry includes the following steps: (1) Raw materials are prepared according to weight percentage; (2) Mix water, inorganic silicate modified resin and modified silica aerogel, disperse and mix well to form a uniform base material; (3) Add the short glass fiber and nano clay dispersion, first shear and disperse, then add the double coupling agent and stir to mix well; (4) Add methyltrimethoxysilane, defoamer and wetting agent to adjust the viscosity of the slurry to 25~30mPa・s and pH value to 9~9.5 to obtain composite slurry.

9. An aerogel insulation felt, characterized in that, The aerogel insulation felt is prepared by sintering the composite slurry as described in any one of claims 1-8 onto the fiber felt.

10. A method for preparing the aerogel insulation felt according to claim 9, characterized in that, The preparation method of the aerogel insulation felt includes the following steps: (1) Pre-impregnate the fiber felt; (2) Place the pre-impregnated fiber felt in an environment with a vacuum degree of -0.08MPa to -0.1MPa and impregnate it with the composite slurry so that the slurry penetrates into the pores of the fiber felt; then, by extrusion, control the amount of slurry coating on the surface of the fiber felt to be 1000~1200g / m²·mm. (3) Sinter the impregnated fiber felt; (4) Surface hydrophobic treatment; (5) Drying is required.

11. The method for preparing aerogel insulation felt according to claim 10, characterized in that, In step (4), a 5% volume concentration of SILRES®BS4004 solution is used as a hydrophobic agent for surface hydrophobic treatment.

12. The aerogel insulation felt according to any one of claims 9-11, characterized in that, The fiber felt is selected from one of the following: glass fiber felt, carbon fiber felt, nickel fiber felt, stainless steel fiber felt, aluminum silicate fiber felt, ceramic fiber felt, alumina fiber felt, basalt fiber felt, and polyacrylonitrile fiber felt.

13. The aerogel insulation felt according to any one of claims 9-12, characterized in that, The thickness of the fiber felt is 0.5-500 mm.

14. The aerogel insulation felt according to any one of claims 9-13, characterized in that, The coating amount of the composite slurry on the surface of the fiber felt is 0.5-50 kg / m. 2 .

15. The composite slurry according to any one of claims 1-3, characterized in that, The raw materials for preparing the modified silica aerogel include: Halloysite nanotubes; Dodecyl methacrylate and / or pentafluorophenyl methacrylate; Silica sol (SiO2 content 25%).

16. The composite slurry as described in claim 15, characterized in that, The raw materials for preparing the modified silica aerogel also include lightweight microspheres.

17. The composite slurry as described in claim 16, characterized in that, The lightweight microspheres include one or more of the following: hollow glass microspheres, hollow silica microspheres, hollow ceramic microspheres, and phenolic resin hollow microspheres.

18. The composite slurry as described in claim 17, characterized in that, The lightweight microspheres have a particle size of 100-350 μm.

19. The composite slurry as described in claim 17, characterized in that, The density of the lightweight microspheres is 0.1-0.4 g / cm³. 3 .

20. The composite slurry according to any one of claims 1-3, characterized in that, The modified silica aerogel was prepared by copolymerizing halloysite nanotubes and silica sol.

21. The composite slurry as described in claim 20, characterized in that, In the modified silica aerogel, the copolymer-modified halloysite nanotubes are connected to the silica sol via Si-O-Si bonds.

22. The composite slurry according to claim 20 or 21, characterized in that, The surface of the copolymer-modified halloysite nanotubes is coated with pentafluorophenyl ester groups and dodecyl ester groups.

23. The composite slurry according to claim 20 or 21, characterized in that, The copolymer-modified halloysite nanotubes were modified with dodecyl methacrylate and pentafluorophenyl methacrylate.

24. The composite slurry according to any one of claims 20-23, characterized in that, The preparation method of the copolymer-modified halloysite nanotubes includes the following steps: adding dodecyl methacrylate and / or pentafluorophenyl methacrylate, organic solvent and halloysite nanotubes into a reaction vessel, adding an initiator, controlling the reaction temperature at 70-80℃, stirring while reacting, reacting for 4-8 hours, cooling, filtering to collect the filter residue, washing, drying, and obtaining copolymer-modified halloysite nanotubes.

25. The composite slurry according to claim 24, characterized in that, The halloysite nanotubes are coupling-modified halloysite nanotubes.

26. The composite slurry according to claim 25, characterized in that, The preparation process of the coupling-modified halloysite nanotubes includes the following steps: adding silane coupling agent, water and pretreated halloysite nanotubes into a reaction vessel, adjusting the pH to 9-10, reacting at 60-80℃ for 2-3 hours, adjusting the pH to neutral, cooling, filtering, washing the filter residue, drying, and obtaining the copolymer-modified halloysite nanotubes.

27. The composite slurry as described in claim 26, characterized in that, The weight ratio of the silane coupling agent, water, and pretreated halloysite nanotubes is 1-1.5:100:9-14.

28. The composite slurry as described in claim 26 or 27, characterized in that, The preparation process of the pretreated halloysite nanotubes includes the following steps: Halloysite nanotubes with a weight ratio of (1:8-10) are mixed with 20wt% urea solution, sonicated, allowed to stand, then 5wt% sulfuric acid solution is added, allowed to stand, filtered, and dried to obtain pretreated halloysite nanotubes; wherein, the weight ratio of sulfuric acid solution to halloysite nanotubes is 5:

1.

29. A method for preparing the composite slurry according to any one of claims 15-28, characterized in that, Includes the following steps: (1) Raw materials are prepared according to weight percentage; (2) Mix water, inorganic silicate modified resin and modified silica aerogel, disperse and mix well to form a uniform base material; (3) Add the short glass fiber and nano clay dispersion, first shear and disperse, then add the double coupling agent and stir to mix well; (4) Add methyltrimethoxysilane, defoamer and wetting agent to adjust the viscosity of the slurry to 25~30mPa・s and pH value to 9~9.5 to obtain composite slurry.

30. An aerogel insulation felt, characterized in that, The aerogel insulation felt is prepared by sintering the composite slurry as described in any one of claims 15-28 onto the fiber felt.

31. A method for preparing the aerogel insulation felt according to claim 30, characterized in that, The preparation method of the aerogel insulation felt includes the following steps: (1) Pre-impregnate the fiber felt; (2) The pre-impregnated fiber felt is placed in an environment with a vacuum degree of -0.08MPa to -0.1MPa and impregnated with the composite slurry so that the composite slurry penetrates into the pores of the fiber felt; then, by extrusion, the amount of slurry coating on the surface of the fiber felt is controlled to be 1000~1200g / m²·mm. (3) Sinter the impregnated fiber felt; (4) Surface hydrophobic treatment; (5) Drying is required.

32. The method for preparing aerogel insulation felt according to claim 31, characterized in that, In step (4), a 5% volume concentration of SILRES®BS4004 solution is used as a hydrophobic agent for surface hydrophobic treatment.

33. The aerogel insulation felt according to any one of claims 30-33, characterized in that, The fiber felt is selected from one of the following: glass fiber felt, carbon fiber felt, nickel fiber felt, stainless steel fiber felt, aluminum silicate fiber felt, ceramic fiber felt, alumina fiber felt, basalt fiber felt, and polyacrylonitrile fiber felt.

34. The aerogel insulation felt according to any one of claims 30-33, characterized in that, The thickness of the fiber felt is 0.5-500 mm.

35. The aerogel insulation felt according to any one of claims 30-34, characterized in that, The coating amount of the composite slurry on the surface of the fiber felt is 0.5-50 kg / m. 2 .

36. The aerogel insulation felt according to any one of claims 30-35, characterized in that, The preparation method of the aerogel thermal insulation felt includes the following steps: coating the surface of the fiber felt with aerogel slurry, allowing it to stand until the fiber felt stably adsorbs the aerogel slurry, and drying it to obtain the aerogel thermal insulation felt.

37. The aerogel insulation felt as described in claims 30-36, characterized in that, The coating amount of the composite slurry on the surface of the fiber felt is 0.5-50 kg / m. 2 .