Fireproof material based on liquid silica gel and glass fiber and preparation method thereof

By combining modified glass fiber with liquid silicone, a nanoscale concave-convex structure and a multi-layered heat insulation network are formed, which solves the problems of softness, thickness and fire resistance limit of existing fireproof materials, and achieves simultaneous improvement in efficient flame retardancy, heat insulation and flexibility.

CN120924040APending Publication Date: 2025-11-11ANHUI SIYAN NEW MATERIAL TECH CO LTD
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Patent Information

Application Number
CN202511006167.3
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-07-21
Publication Date
2025-11-11

AI Technical Summary

Technical Problem

Existing fireproof materials have shortcomings in terms of flexibility, thickness, fire resistance limit, bonding strength, impact resistance, and weather resistance, resulting in short service life and rapid performance degradation.

Method used

By modifying glass fiber, nano-seeds, nano-silica, and ammonium polyphosphate are added to form a nanoscale concave-convex structure, which enhances the bonding force between the fiber and liquid silicone. Furthermore, a multi-layer heat insulation structure is formed through cyclopentadiene crosslinking, thereby improving the flame retardancy and flexibility of the material.

Benefits of technology

This achieves improved high-efficiency flame retardancy and heat insulation properties, increased softness, reduced thermal conductivity, extended service life, and significantly improved overall performance of the material.

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Abstract

The invention relates to a fireproof material based on liquid silica gel and glass fiber and a preparation method thereof, and belongs to the technical field of fireproof materials, the fireproof material is prepared from the following raw materials: 90-120 parts of liquid silica gel, 20-30 parts of modified glass fiber, 5-10 parts of hydroxyl silicone oil, 5-10 parts of fumed silica, 0.5-1 part of a cross-linking agent and 0.01-0.02 part of a platinum catalyst; the modified glass fibers are prepared by cleaning glass fibers, mixing the cleaned glass fibers with carboxymethyl cellulose, adding nano seed crystal, heating, spraying at high pressure, carrying out alkali etching, impregnating with a silane coupling agent, impregnating with a cyclopentadiene solution containing nano silicon dioxide and ammonium polyphosphate, and drying. According to the invention, the surface area and activity of the glass fiber are increased through the nanocrystalline seed, and then the silane coupling agent is utilized to modify and reinforce the combination with the liquid silica gel; and finally, nano silicon dioxide and ammonium polyphosphate are synergistically flame-retardant, and the flexibility is improved by regrowth of cyclopentadiene in liquid silica gel. The flame-retardant, flexible and heat-insulating properties are good, and the material is suitable for fireproof materials.
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Description

Technical Field

[0001] This invention belongs to the field of fireproof materials technology, specifically relating to a fireproof material based on liquid silicone and glass fiber and its preparation method. Background Technology

[0002] Currently produced fire-resistant materials are composite fire-resistant materials that use glass fiber and liquid silicone as separate layers. This involves coating both sides of a glass fiber cloth with silicone slurry and then heating it until the silicone is completely cured. For example, CN202411668638.2 discloses an anti-aging fire-resistant cloth for building materials and its preparation method. However, its flexibility is limited by the glass fiber cloth, and because it is a composite layer structure, its thickness is relatively large, limiting its application areas.

[0003] Fireproof cloths made by mixing liquid silicone and glass fiber also have several drawbacks. For example, silicone cannot withstand temperatures exceeding 300°C for extended periods; it decomposes and releases toxic gases at high temperatures, leading to structural damage and a fire resistance limit often less than 1 hour. The bonding between liquid silicone and inorganic glass fiber is weak, making it prone to delamination. Furthermore, the material has poor impact resistance and flexibility, easily cracking and creating fireproof gaps during use. Silicone is also susceptible to aging due to UV radiation and humidity, while glass fiber may experience alkali corrosion, resulting in a typical service life of only 3-5 years and rapid long-term performance degradation. Summary of the Invention

[0004] The purpose of this invention is to provide a fire-retardant material based on liquid silicone and glass fiber and its preparation method in order to solve the above-mentioned problems.

[0005] The present invention achieves the above objectives through the following technical solutions:

[0006] A fire-retardant material based on liquid silicone and glass fiber, wherein, by weight, the raw materials for preparing the fire-retardant material include: 90-120 parts of liquid silicone, 20-30 parts of modified glass fiber, 5-10 parts of hydroxyl silicone oil, 5-10 parts of fumed silica, 0.5-1 parts of crosslinking agent, and 0.01-0.02 parts of platinum catalyst;

[0007] The modified glass fiber is prepared as follows:

[0008] (1) Ordinary glass fiber is cleaned and mixed with carboxymethyl cellulose of equal mass, and then heated. During the heating process, nano crystal seeds are added and the heating is continued. Glass fiber is obtained by high-pressure spraying.

[0009] (2) The glass fiber is uniformly dispersed in an alkaline solution for etching, cleaned and dried, and then immersed in a silane coupling agent for impregnation treatment;

[0010] (3) The impregnated glass fiber is placed in a cyclopentadiene solution containing nano-silica and ammonium polyphosphate, and after washing and drying, modified glass fiber is obtained.

[0011] As a further optimization of the present invention, in step (1), the heating treatment is as follows: the temperature is raised to 300-400℃ in the first stage, nano-crystal seeds are added, and then raised to 1200-1300℃ and held for 0.5-1h. Glass fibers are obtained by high-pressure spraying and then washed with ethanol and deionized water after cooling.

[0012] As a further optimization of the present invention, the nanocrystal seed is one of nano-titanium dioxide, nano-zirconium dioxide, and nano-silicon dioxide.

[0013] As a further optimization of the present invention, in step (2), the glass fiber is uniformly dispersed in a sodium hydroxide alkaline solution at 40-50°C for etching.

[0014] As a further optimization of the present invention, in step (2), the silane coupling agent is one of KH-550, KH-560, KH-570, and KH-792, and the impregnation time is 12-48h.

[0015] As a further optimization of the present invention, in step (3), a suspension containing 30-40% nano-silica is mixed with a solution containing 10-20% ammonium polyphosphate at a mass ratio of 1:1-3:1, stirred at 60-80°C for 2-4 hours, and obtained nano-silica particles loaded with ammonium polyphosphate after centrifugation, washing and drying; the nano-silica particles loaded with ammonium polyphosphate are uniformly dispersed in a cyclopentadiene solution at a temperature of 0-20°C.

[0016] As a further optimization of the present invention, in step (3), the impregnated glass fiber is completely immersed in the cyclopentadiene solution, stirred at 0-20°C for 2-4 hours, and then cleaned and dried to obtain modified glass fiber.

[0017] As a further optimization of the present invention, the liquid silicone is vinyl polysiloxane.

[0018] As a further optimization of the present invention, the crosslinking agent is one of methylphenyl hydrogen-containing polysiloxane, methyl hydrogen-containing polysiloxane, and methyl hydrogen-containing silicone resin.

[0019] The present invention also provides a method for preparing the above-mentioned fire-retardant material based on liquid silicone and glass fiber, comprising the following steps:

[0020] (1) Place the liquid silica gel into a container and stir it. Add modified glass fiber, hydroxyl silicone oil and fumed silica to it. After uniform dispersion, add crosslinking agent and platinum catalyst. Stir at high speed until uniform and let stand to obtain liquid silica gel raw material.

[0021] (2) The liquid silicone raw material is put into the molding equipment to obtain the fireproof material product; wherein the molding equipment includes one of injection molding, casting molding, coating / impregnation molding or calendering molding.

[0022] The beneficial effects of this invention are as follows:

[0023] In this invention, by adding nanocrystal seeds during the processing of glass fibers, the nanocrystal seeds can act as nucleation points during high-temperature processing, promoting the formation of nanoscale uneven structures or whisker-like protrusions on the surface of the glass fibers, thereby increasing the specific surface area. The glass fibers modified with nanocrystal seeds have higher surface activity and react more fully with silane coupling agents, forming stronger "molecular bridges" between the fibers and liquid silica gel.

[0024] In this invention, nano-silica and ammonium polyphosphate synergistically retard flame, promote char formation and enhance char layer stability, thereby improving flame retardant efficiency. Cyclopentadiene stably disperses the two at low temperatures, preventing agglomeration and premature decomposition. Its double bonds can react with coupling agents to enhance the bond between fibers and the matrix. The resulting composite layer combines flame retardancy and flexibility, improving the material's elongation at break and softness while reducing thermal conductivity. Cyclopentadiene, as a crosslinking component, is loaded onto glass fibers. During the preparation process, crosslinking occurs between the ends of the glass fibers, similar to "regeneration," which increases the material's flexibility and meets the requirements of fire-resistant materials.

[0025] In this invention, a silane coupling agent improves the compatibility between glass fiber and liquid silicone, while hydroxyl silicone oil regulates the flexibility of the liquid silicone system, synergistically enhancing elongation at break and softness. Glass fiber, fumed silica, and nano-silica form a multi-layered thermal insulation structure, hindering heat conduction and enhancing the thermal insulation effect. The synergistic effect of flame retardancy and thermal insulation makes it highly suitable for fire-resistant materials. Detailed Implementation

[0026] The present application will now be described in further detail. It should be noted that the following specific embodiments are only used to further illustrate the present application and should not be construed as limiting the scope of protection of the present application. Those skilled in the art can make some non-essential improvements and adjustments to the present application based on the above application content.

[0027] 1. Explanation

[0028] At least one embodiment of this invention discloses a fire-retardant material based on liquid silicone and glass fiber. By weight, the raw materials for preparing the fire-retardant material include: 90-120 parts of liquid silicone, 20-30 parts of modified glass fiber, 5-10 parts of hydroxyl silicone oil, 5-10 parts of fumed silica, 0.5-1 parts of crosslinking agent, and 0.01-0.02 parts of platinum catalyst.

[0029] Liquid silicone (vinyl polysiloxane) was sourced from Fengyang Jiasong New Material Technology Co., Ltd.; hydroxyl silicone oil and platinum catalyst were purchased from Anhui Aiyota Silicon Oil Co., Ltd.; and nano silica and fumed silica were purchased from Anhui Fengyang Saijiyuan Inorganic Materials Co., Ltd.

[0030] The crosslinking agent in this invention is one of methylphenyl hydrogen-containing polysiloxane, methyl hydrogen-containing polysiloxane, and methyl hydrogen-containing silicone resin. The following experiments use methyl hydrogen-containing polysiloxane.

[0031] At least one embodiment of the present invention discloses a method for preparing modified glass fibers, as detailed below:

[0032] (1) Ordinary glass fiber is cleaned and mixed with carboxymethyl cellulose by mass, and then heated. In the first stage, the temperature is raised to 300-400℃, and 5% of the total system mass of nano-crystal seeds are added. The temperature is then raised to 1200-1300℃ and held for 0.5-1h. Glass fiber is obtained by high-pressure spraying. After cooling, it is washed with ethanol and deionized water. The nano-crystal seeds are one of nano-titanium dioxide, nano-zirconium dioxide, and nano-silica.

[0033] (2) The glass fiber is uniformly dispersed in an alkaline solution for etching, cleaned and dried, and then immersed in a silane coupling agent for impregnation treatment.

[0034] The silane coupling agent is one of KH-550, KH-560, KH-570, and KH-792, with KH-570 being preferred.

[0035] (3) A suspension containing 30-40% nano silica and a solution containing 10-20% ammonium polyphosphate are mixed at a mass ratio of 1:1-3:1 and stirred at 60-80℃ for 2-4 hours. After centrifugation, washing and drying, nano silica particles loaded with ammonium polyphosphate are obtained. At 0-20℃, the nano silica particles loaded with ammonium polyphosphate are uniformly dispersed in a cyclopentadiene solution. The impregnated glass fiber is completely immersed in the cyclopentadiene solution and stirred at 0-20℃ for 2-4 hours. After washing and drying, modified glass fiber is obtained.

[0036] Suspension containing 30-40% nano-silica:

[0037] Nano-silica is soaked in dilute hydrochloric acid (1%-5%) to remove residual metal ions (such as Na+) from the surface. + Ca 2+ Remove impurities such as organic matter and increase the surface hydroxyl density; vacuum dry the activated nano-silica at 80-120℃ for 4-6 hours to remove moisture; then disperse it in deionized water by ultrasonic dispersion at 300-500W for 30-60 minutes to form a stable nano-SiO2 suspension (concentration 30-40%).

[0038] Solution containing 10-20% ammonium polyphosphate:

[0039] Dissolve ammonium polyphosphate (APP) in deionized water (concentration 10%-20%), heat to 50-60℃ to promote dissolution, and form a clear APP solution.

[0040] At least one embodiment of the present invention discloses a method for preparing fire-retardant materials, comprising the following steps:

[0041] (1) Place the liquid silica gel into a container and stir it. Add modified glass fiber, hydroxyl silicone oil and fumed silica to it. After uniform dispersion, add crosslinking agent and platinum catalyst. Stir at high speed until uniform and let stand to obtain liquid silica gel raw material.

[0042] (2) The liquid silicone raw material is put into the molding equipment to obtain the fireproof material product; wherein the molding equipment includes one of injection molding, casting molding, coating / impregnation molding or calendering molding, and the specific molding equipment is selected according to the actual shape of the product.

[0043] Unless otherwise specified, all methods used in this invention are conventional methods known to those skilled in the art, and all reagents and materials used are commercially available products.

[0044] 2. Methods

[0045] Example 1

[0046] The raw materials for preparing the fireproof material in this embodiment, by weight, include: 100 parts liquid silicone, 30 parts modified glass fiber, 10 parts hydroxyl silicone oil, 8 parts fumed silica, 0.5 parts crosslinking agent, and 0.01 parts platinum catalyst.

[0047] The preparation method of modified glass fiber is as follows:

[0048] (1) After cleaning ordinary glass fiber, it is mixed with carboxymethyl cellulose of equal mass and subjected to heat treatment. The temperature is raised to 360℃ (±10℃) in the first stage, nano titanium dioxide seed crystals are added, and then raised to 1200℃ (±50℃) and held for 1 hour. Glass fiber is obtained by high-pressure spraying and then washed with ethanol and deionized water after cooling.

[0049] (2) The glass fiber was uniformly dispersed in a sodium hydroxide alkaline solution at 40°C for etching. After cleaning and drying, it was immersed in silane coupling agent KH-570 for immersion treatment for 12 hours.

[0050] (3) Mix a suspension containing 30-40% nano silica with a solution containing 10-20% ammonium polyphosphate at a mass ratio of 1:1, stir at 60-80℃ for 2 hours, centrifuge, wash and dry to obtain nano silica particles loaded with ammonium polyphosphate; uniformly disperse the nano silica particles loaded with ammonium polyphosphate in a cyclopentadiene solution at a temperature not exceeding 20℃; completely immerse the impregnated glass fiber in the cyclopentadiene solution, stir at a temperature not exceeding 20℃ for 2 hours, wash and dry to obtain modified glass fiber.

[0051] The preparation method of fire-resistant materials includes the following steps:

[0052] (1) Place the liquid silicone into a high-speed shear machine for stirring, add modified glass fiber, hydroxyl silicone oil and fumed silica, disperse evenly, then add crosslinking agent and platinum catalyst, stir evenly at high speed and let stand to obtain liquid silicone raw material.

[0053] (2) The liquid silicone raw material is put into the coating molding equipment to obtain the finished fireproof material.

[0054] Example 2

[0055] In the preparation method of modified glass fiber, the nanocrystal seed in step (1) is replaced with nano-zirconia, and the rest is the same as in Example 1.

[0056] Example 3

[0057] In the preparation method of modified glass fiber, the nanocrystal seeds in step (1) are replaced with nano-silica, and the rest is the same as in Example 1.

[0058] Comparative Example 1

[0059] The raw materials for preparing the fireproof material in this comparative example, by weight, include: 100 parts liquid silicone, 30 parts ordinary glass fiber, 10 parts hydroxyl silicone oil, 8 parts fumed silica, 0.5 parts crosslinking agent, and 0.01 parts platinum catalyst.

[0060] Comparative Example 2

[0061] The raw materials for preparing the fireproof material in this comparative example, by weight, include: 100 parts liquid silicone, 30 parts glass fiber, 10 parts hydroxyl silicone oil, 8 parts fumed silica, 0.5 parts crosslinking agent, and 0.01 parts platinum catalyst.

[0062] The preparation method of glass fiber one is as follows:

[0063] (1) Ordinary glass fiber was cleaned and mixed with carboxymethyl cellulose of equal mass, and then heated. The temperature was raised to 360℃ (±10℃) in the first stage, then raised to 1200℃ (±50℃) and held for 1 hour. Glass fiber was obtained by high-pressure spraying and then washed with ethanol and deionized water after cooling.

[0064] (2) The glass fiber was uniformly dispersed in a sodium hydroxide alkaline solution at 40°C for etching. After cleaning and drying, it was immersed in silane coupling agent KH-570 for immersion treatment for 12 hours.

[0065] (3) Mix a suspension containing 30-40% nano silica with a solution containing 10-20% ammonium polyphosphate at a mass ratio of 1:1, stir at 60-80℃ for 2 hours, centrifuge, wash and dry to obtain nano silica particles loaded with ammonium polyphosphate; uniformly disperse the nano silica particles loaded with ammonium polyphosphate in a cyclopentadiene solution at a temperature not exceeding 20℃; completely immerse the impregnated glass fiber in the cyclopentadiene solution, stir at a temperature not exceeding 20℃ for 2 hours, wash and dry to obtain glass fiber one.

[0066] The preparation method of the fireproof material is the same as in Example 1.

[0067] Comparative Example 3

[0068] The raw materials for preparing the fireproof material in this comparative example, by weight, include: 100 parts liquid silicone, 30 parts glass fiber, 10 parts hydroxyl silicone oil, 8 parts fumed silica, 0.5 parts crosslinking agent, and 0.01 parts platinum catalyst.

[0069] The preparation method of glass fiber II is as follows:

[0070] (1) After cleaning ordinary glass fiber, it is mixed with carboxymethyl cellulose of equal mass and subjected to heat treatment. The temperature is raised to 360℃ (±10℃) in the first stage, nano titanium dioxide seed crystals are added, and then raised to 1200℃ (±50℃) and held for 1 hour. Glass fiber is obtained by high-pressure spraying and then washed with ethanol and deionized water after cooling.

[0071] (2) A suspension containing 30-40% nano silica is mixed with a solution containing 10-20% ammonium polyphosphate at a mass ratio of 1:1. The mixture is stirred at 60-80℃ for 2 hours, and after centrifugation, washing and drying, nano silica particles loaded with ammonium polyphosphate are obtained. The nano silica particles loaded with ammonium polyphosphate are uniformly dispersed in a cyclopentadiene solution at a temperature not exceeding 20℃. Glass fibers are completely immersed in the cyclopentadiene solution and stirred at a temperature not exceeding 20℃ for 2 hours. After washing and drying, glass fiber 2 is obtained.

[0072] The preparation method of the fireproof material is the same as in Example 1.

[0073] Comparative Example 4

[0074] The raw materials for preparing the fireproof material in this comparative example, by weight, include: 100 parts liquid silicone, 30 parts glass fiber, 10 parts hydroxyl silicone oil, 8 parts fumed silica, 0.5 parts crosslinking agent, and 0.01 parts platinum catalyst.

[0075] The preparation method of glass fiber 3 is as follows:

[0076] (1) After cleaning ordinary glass fiber, it is mixed with carboxymethyl cellulose of equal mass and subjected to heat treatment. The temperature is raised to 360℃ (±10℃) in the first stage, nano titanium dioxide seed crystals are added, and then raised to 1200℃ (±50℃) and held for 1 hour. Glass fiber is obtained by high-pressure spraying and then washed with ethanol and deionized water after cooling.

[0077] (2) The glass fiber was uniformly dispersed in a sodium hydroxide alkaline solution at 40°C for etching. After cleaning and drying, it was immersed in silane coupling agent KH-570 for immersion treatment for 12 hours.

[0078] (3) At a temperature not exceeding 20°C, the nano-silica particles are uniformly dispersed in a cyclopentadiene solution (30-40%); the impregnated glass fiber is completely immersed in the cyclopentadiene solution, stirred for 2 hours at a temperature not exceeding 20°C, and then washed and dried to obtain glass fiber 3.

[0079] The preparation method of the fireproof material is the same as in Example 1.

[0080] Comparative Example 5

[0081] The raw materials for preparing the fireproof material in this comparative example, by weight, include: 100 parts liquid silicone, 30 parts glass fiber, 10 parts hydroxyl silicone oil, 8 parts fumed silica, 0.5 parts crosslinking agent, and 0.01 parts platinum catalyst.

[0082] The preparation method of glass fiber 4 is as follows:

[0083] (1) After cleaning ordinary glass fiber, it is mixed with carboxymethyl cellulose of equal mass and subjected to heat treatment. The temperature is raised to 360℃ (±10℃) in the first stage, nano titanium dioxide seed crystals are added, and then raised to 1200℃ (±50℃) and held for 1 hour. Glass fiber is obtained by high-pressure spraying and then washed with ethanol and deionized water after cooling.

[0084] (2) The glass fiber was uniformly dispersed in a sodium hydroxide alkaline solution at 40°C for etching. After cleaning and drying, it was immersed in silane coupling agent KH-570 for immersion treatment for 12 hours.

[0085] (3) At a temperature not exceeding 20°C, a solution containing 10-20% ammonium polyphosphate is uniformly dispersed in a cyclopentadiene solution (30-40%); the impregnated glass fiber is completely immersed in the cyclopentadiene solution, stirred for 2 hours at a temperature not exceeding 20°C, and then washed and dried to obtain glass fiber four.

[0086] The preparation method of the fireproof material is the same as in Example 1.

[0087] Comparative Example 6

[0088] The raw materials for preparing the fireproof material in this comparative example, by weight, include: 100 parts liquid silicone, 30 parts glass fiber, 10 parts hydroxyl silicone oil, 8 parts fumed silica, 0.5 parts crosslinking agent, and 0.01 parts platinum catalyst.

[0089] The preparation method of modified glass fiber is as follows:

[0090] (1) After cleaning ordinary glass fiber, it is mixed with carboxymethyl cellulose of equal mass and subjected to heat treatment. The temperature is raised to 360℃ (±10℃) in the first stage, nano titanium dioxide seed crystals are added, and then raised to 1200℃ (±50℃) and held for 1 hour. Glass fiber is obtained by high-pressure spraying and then washed with ethanol and deionized water after cooling.

[0091] (2) The glass fiber was uniformly dispersed in a sodium hydroxide alkaline solution at 40°C for etching. After cleaning and drying, it was immersed in silane coupling agent KH-570 for immersion treatment for 12 hours.

[0092] (3) A suspension containing 30-40% nano silica and a solution containing 10-20% ammonium polyphosphate are mixed at a mass ratio of 1:1 and stirred at 60-80℃ for 2 hours. After centrifugation, washing and drying, nano silica particles loaded with ammonium polyphosphate are obtained. At room temperature, the nano silica particles loaded with ammonium polyphosphate are uniformly dispersed in deionized water. The impregnated glass fiber is completely immersed in the above deionized water, stirred at room temperature for 2 hours, washed and dried to obtain glass fiber five.

[0093] The preparation method of the fireproof material is the same as in Example 1.

[0094] III. Performance Testing

[0095] The fire-resistant materials prepared in Examples 1-3 and Comparative Examples 1-6 were cut to appropriate sizes as test samples and subjected to the following tests:

[0096] Flame retardancy: Refer to standard UL94-2009; each test sample was heated to 1000℃ at a rate of 10℃ / min and held for 1 hour, and the change in ablation mass was detected.

[0097] Thermal conductivity: Refer to standard ASTM / D5470; the thickness of each test sample is set to 5 mm.

[0098] Tensile strength: The elongation at break of each test sample was measured using a tensile testing machine, and the test method was in accordance with standard GB / T528-2009.

[0099] The test results are shown in the table below:

[0100] Group Change in ablation quality / % Thermal conductivity (W / (m·K)) Elongation at break / % Example 1 40.5 0.22 540 Example 2 41.3 0.23 545 Example 3 41.0 0.21 540 Comparative Example 1 43.2 0.30 420 Comparative Example 2 41.9 0.28 490 Comparative Example 3 41.6 0.26 510 Comparative Example 4 45.5 0.24 515 Comparative Example 5 41.3 0.24 530 Comparative Example 6 42.0 0.27 460

[0101] The fireproof material prepared by this invention has good flame retardancy and elongation at break, and has a low thermal conductivity, making it suitable for fireproof materials.

[0102] The ablation mass change rate of Examples 1-3 was 40.5%-41.3%, significantly lower than the 41.6%-45.5% of the comparative examples. The nanostructures (such as whiskers) formed by the nano-titanium dioxide seeds on the glass fiber surface increase the specific surface area and enhance the bonding force with the silane coupling agent, making the loaded nano-silica and ammonium polyphosphate more robust; the two form a silicon-phosphorus-carbon composite layer at high temperature, which effectively blocks oxygen and heat transfer and reduces substrate ablation.

[0103] The thermal conductivity of Examples 1-3 was 0.21-0.23 W / (m·K), significantly lower than the 0.24-0.30 W / (m·K) of the comparative examples. This indicates that the modified glass fiber, fumed silica, and liquid silicone in this invention form a multi-layered thermal insulation network. The porous structure of the nano-silica intertwines with the glass fiber, extending the heat conduction path; the polymer layer after cyclopentadiene curing further reduces the heat transfer efficiency.

[0104] The elongation at break in the embodiment was 540%-545%, far exceeding the 420%-530% of the comparative example. The silane coupling agent (KH-570) forms strong chemical bonds between the glass fiber and the liquid silicone, improving stress transmission; the hydroxyl silicone oil regulates the crosslinking density of the system, inhibiting embrittlement caused by rigid particles; the flexibility of the cyclopentadiene cured layer buffers stress concentration and prevents crack propagation.

[0105] This invention achieves simultaneous improvements in flame retardancy (reducing ablation rate by 10%-15%), thermal conductivity (reducing by 20%-30%), and flexibility (increasing by 10%-30%) through a triple mechanism of "nanostructure regulation - flame retardant synergy - cross-linking regeneration", resulting in significant overall performance.

[0106] The embodiments described above are merely examples of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention.

Claims

1. A fire-retardant material based on liquid silicone and glass fiber, characterized in that, The raw materials for preparing the fireproof material, by weight, include: 90-120 parts of liquid silicone, 20-30 parts of modified glass fiber, 5-10 parts of hydroxyl silicone oil, 5-10 parts of fumed silica, 0.5-1 parts of crosslinking agent, and 0.01-0.02 parts of platinum catalyst. The modified glass fiber is prepared as follows: (1) Ordinary glass fiber is cleaned and mixed with carboxymethyl cellulose of equal mass, and then heated. During the heating process, nano crystal seeds are added and the heating is continued. Glass fiber is obtained by high-pressure spraying. (2) The glass fiber is uniformly dispersed in an alkaline solution for etching, cleaned and dried, and then immersed in a silane coupling agent for impregnation treatment; (3) The impregnated glass fiber is placed in a cyclopentadiene solution containing nano-silica and ammonium polyphosphate, and after washing and drying, modified glass fiber is obtained.

2. The fire-retardant material based on liquid silicone and glass fiber according to claim 1, characterized in that, In step (1), the heating treatment is as follows: the temperature is raised to 300-400℃ in the first stage, nano-crystal seeds are added, and then the temperature is raised to 1200-1300℃ and maintained for 0.5-1h. Glass fibers are obtained by high-pressure spraying and then washed with ethanol and deionized water after cooling.

3. A fire-retardant material based on liquid silicone and glass fiber according to claim 2, characterized in that, The nanocrystal seed is one of nano-titanium dioxide, nano-zirconium dioxide, or nano-silicon dioxide.

4. The fire-retardant material based on liquid silicone and glass fiber according to claim 1, characterized in that, In step (2), the glass fiber is uniformly dispersed in a sodium hydroxide alkaline solution at 40-50°C for etching.

5. A fire-retardant material based on liquid silicone and glass fiber according to claim 4, characterized in that, In step (2), the silane coupling agent is one of KH-550, KH-560, KH-570, and KH-792, and the impregnation time is 12-48h.

6. A fire-retardant material based on liquid silicone and glass fiber according to claim 1, characterized in that, In step (3), a suspension containing 30-40% nano silica is mixed with a solution containing 10-20% ammonium polyphosphate at a mass ratio of 1:1-3:1, stirred at 60-80℃ for 2-4 hours, and obtained nano silica particles loaded with ammonium polyphosphate after centrifugation, washing and drying; the nano silica particles loaded with ammonium polyphosphate are uniformly dispersed in a cyclopentadiene solution at a temperature of 0-20℃.

7. A fire-retardant material based on liquid silicone and glass fiber according to claim 6, characterized in that, In step (3), the impregnated glass fiber is completely immersed in the cyclopentadiene solution, stirred at 0-20°C for 2-4 hours, and then cleaned and dried to obtain modified glass fiber.

8. A fire-retardant material based on liquid silicone and glass fiber according to claim 1, characterized in that, The liquid silicone is vinyl polysiloxane.

9. A fire-retardant material based on liquid silicone and glass fiber according to claim 1, characterized in that, The crosslinking agent is one of methylphenyl hydrogen-containing polysiloxane, methyl hydrogen-containing polysiloxane, and methyl hydrogen-containing silicone resin.

10. A method for preparing a fire-retardant material based on liquid silicone and glass fiber as described in any one of claims 1-9, characterized in that, Includes the following steps: (1) Place the liquid silica gel into a container and stir it. Add modified glass fiber, hydroxyl silicone oil and fumed silica to it. After uniform dispersion, add crosslinking agent and platinum catalyst. Stir at high speed until uniform and let stand to obtain liquid silica gel raw material. (2) The liquid silicone raw material is put into the molding equipment to obtain the fireproof material product; wherein the molding equipment includes one of injection molding, casting molding, coating / impregnation molding or calendering molding.

Citation Information

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