Preparation method of modified siloxyl glass fiber, preparation method and application of flame-retardant thermal-insulation fireproof fabric

Abstract

The application discloses a preparation method of modified siloxyl glass fiber, a preparation method and application of a flame-retardant heat-insulating fireproof fabric, and belongs to the technical field of fireproof heat-insulating materials. The preparation method provided by the application modifies the siloxyl glass fiber through the synergistic effect of glass micro and silica aerogel, gives the modified siloxyl glass fiber excellent heat-retention and heat-insulation performance and hydrophobicity, then weaves the modified siloxyl glass fiber into the flame-retardant heat-insulating fireproof fabric through the warp two-dimensional multi-dimensional weaving mode, and obtains a sandwich structure with aramid fibers as upper and lower surface layers and the modified siloxyl glass fiber as the inner layer, so that the flame-retardant heat-insulating fireproof fabric has excellent heat-insulation and fireproof performance and stability, and can be widely applied to fire-fighting clothes.

Description

Technical Field

[0001] This application belongs to the technical field of heat insulation and fireproof materials, and particularly relates to a method for preparing modified silica-oxygenated glass fiber, a method for preparing flame-retardant heat insulation and fireproof fabric, and their application. Background Technology

[0002] In firefighting and rescue operations, fire suits effectively protect firefighters from heat radiation and flames, ensuring their safety. However, traditional fire suits are typically made from a cotton base with flame-retardant finishing, often resulting in bulkiness and poor comfort. Therefore, there is a need to develop comfortable, lightweight fabrics with excellent flame-retardant and heat-insulating properties to improve the overall performance of fire suits.

[0003] The prior art with application publication number CA 110528118 A discloses a method for preparing fireproof, soundproof and heat-insulating fabric. It uses a binder mixed with hydrophobic SiO2 aerogel particles to bond and press the base fabric, heat insulation layer and fireproof outer layer in sequence to obtain a fireproof and heat-insulating fabric with excellent fireproof performance.

[0004] However, the above-mentioned method for preparing fireproof and heat-insulating fabric has the following problems: First, the fabric achieves heat insulation by isolating itself from oxygen through a hyperbranched siloxane structure with maleimide-terminated ends, resulting in poor heat insulation and protection effects; second, the fabric is bonded and pressed by introducing an adhesive, which is prone to falling off, leading to poor protective stability; and third, the fabric does not have hydrophobic and breathable properties, resulting in poor comfort. Summary of the Invention

[0005] This application discloses a method for preparing modified silica-oxygenated glass fiber, a method for preparing flame-retardant and heat-insulating fireproof fabric, and their applications, aiming to solve the technical problems of poor protective effect, poor protective stability, and poor comfort of existing fireproof and heat-insulating fabrics.

[0006] To achieve the above objectives, the technical solution of this application is:

[0007] The first aspect of this application provides a method for preparing modified silica-oxygenated glass fibers, the method comprising:

[0008] Glass microspheres and silica aerogel are added to an adhesive solution of 5-20 wt% to obtain a high-temperature heat-insulating coating.

[0009] Silicon-oxygenated glass fibers are immersed in an alkaline solution for treatment to obtain surface-modified silicon-oxygenated glass fibers;

[0010] After immersing the surface-modified silica-oxygenated glass fiber in the high-temperature heat-insulating coating, it is dried to obtain modified silica-oxygenated glass fiber.

[0011] Preferably, in conjunction with the first aspect, the adhesive solution comprises a high-temperature organosilicon resin dissolved in cyclohexane.

[0012] Preferably, in conjunction with the first aspect, the mass ratio of the glass microspheres to the silica aerogel is 1:1 to 4:1.

[0013] Preferably, in conjunction with the first aspect, the drying temperature is 100-120℃ and the time is 1-2 minutes.

[0014] The second aspect of this application provides modified silica-oxygenated glass fibers prepared by the method described in the first aspect.

[0015] The third aspect of this application provides the application of the modified silica-oxygenated glass fiber described in the second aspect in the preparation of flame-retardant, heat-insulating, and fire-resistant fabrics.

[0016] The fourth aspect of this application provides a method for preparing the flame-retardant, heat-insulating, and fire-resistant fabric described in the third aspect. The method includes: using aramid fibers as warp threads for heddling, odd-numbered weft threads as aramid fibers, and even-numbered weft threads as modified silica-oxygenated glass fibers, and weaving in a double-layer multi-dimensional weaving manner to obtain the flame-retardant, heat-insulating, and fire-resistant fabric.

[0017] In conjunction with the fourth aspect, preferably, the aramid fiber includes one or a combination of aramid 1314 fiber and aramid 1414 fiber.

[0018] The fifth aspect of this application provides a method for preparing the flame-retardant, heat-insulating, and fire-resistant fabric, wherein the flame-retardant, heat-insulating, and fire-resistant fabric is a sandwich structure comprising an aramid fiber as the upper surface layer and a lower surface layer disposed between the modified silica-oxygenated glass fiber of claim 6.

[0019] The sixth aspect of this application provides the use of the flame-retardant, heat-insulating, and fire-resistant fabric described in the fifth aspect in the preparation of fire-fighting clothing.

[0020] Compared with the prior art, the advantages or beneficial effects of the embodiments of this application include at least the following:

[0021] The preparation method provided in this application modifies silica-oxygenated glass fibers through the synergistic effect of glass microspheres and silica aerogel. On the one hand, it can effectively improve the hydrophobic properties of the prepared modified silica-oxygenated glass fibers, so that the fire suit will not swell when exposed to water, thereby improving its comfort. On the other hand, it can effectively reduce the thermal conductivity and density of the prepared modified silica-oxygenated glass fibers, thereby significantly improving the thermal insulation performance of the modified silica-oxygenated glass fibers. The prepared modified silica-oxygenated glass fibers improve the thermal resistance of the modified silica-oxygenated glass fibers by inhibiting heat conduction, blocking heat convection, and blocking heat radiation, thereby improving the flame retardant and heat insulation effect of the fire suit. Attached Figure Description

[0022] To more clearly illustrate the technical solutions of the embodiments of this application, the accompanying drawings used in the description of the embodiments will be briefly introduced below. Obviously, the accompanying drawings described below are only some embodiments recorded in this application. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.

[0023] Figure 1 A fiber weave diagram of the flame-retardant, heat-insulating, and fire-resistant fabric prepared according to the embodiments of this application;

[0024] Figure 2 A schematic diagram of the process for preparing Al-modified silica-oxygenated glass fibers according to an embodiment of this application;

[0025] Figure 3 Scanning electron microscope image of Al-modified silica-oxygenated glass fibers prepared for embodiments of this application;

[0026] Figure 4 A scanning electron microscope image of a planar surface of the A1-flame-retardant, heat-insulating, and fire-resistant fabric prepared for an embodiment of this application;

[0027] Figure 5 Scanning electron microscope image of the cross section of the A1-flame-retardant, heat-insulating, and fireproof fabric prepared for the embodiments of this application;

[0028] Figure 6 DTG diagram of the A1-flame-retardant, heat-insulating, and fireproof fabric prepared according to the embodiments of this application. Detailed Implementation

[0029] The technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some, not all, of the embodiments of this application. All other embodiments obtained by those skilled in the art based on the embodiments of this application without creative effort are within the scope of protection of this application.

[0030] In the following description of this embodiment, the term "and / or" is used to describe the association relationship between related objects, indicating that three relationships can exist. For example, A and / or B can represent: A existing alone, B existing alone, and A and B existing simultaneously. A and B can be singular or plural. The character " / " generally indicates that the preceding and following related objects have an "or" relationship.

[0031] In the following description of this embodiment, the term "at least one" means one or more, and "more than one" means two or more. "At least one of the following" or similar expressions refer to any combination of these items, including any combination of single or multiple items. For example, "at least one of a, b, or c", or "at least one of a, b, and c", can both mean: a, b, c, ab (i.e., a and b), ac, bc, or abc, where a, b, and c can be single or multiple.

[0032] Those skilled in the art should understand that, in the following description of the embodiments of this application, the sequence of numbers does not imply the order of execution. Some or all steps may be executed in parallel or sequentially. The execution order of each process should be determined by its function and internal logic, and should not constitute any limitation on the implementation process of the embodiments of this application.

[0033] The terminology used in the embodiments of this application is for the purpose of describing particular embodiments only and is not intended to be limiting of this application. The singular forms "a" and "the" as used in the embodiments of this application and the appended claims are also intended to include the plural forms, unless the context clearly indicates otherwise.

[0034] It should be noted that all raw materials and reagents in the embodiments of this application were purchased from the market or prepared according to conventional methods known to those skilled in the art. For example, organosilicon resin 908, cyclohexane, glass microspheres, and silica aerogel were all purchased from the market or prepared according to conventional methods known to those skilled in the art.

[0035] In a first aspect, embodiments of this application provide a method for preparing modified silica-oxygenated glass fibers, the method comprising:

[0036] Glass microspheres and silica aerogel are added to an adhesive solution of 5-20 wt% to obtain a high-temperature heat-insulating coating.

[0037] Silicon-oxygenated glass fibers are immersed in an alkaline solution for treatment to obtain surface-modified silicon-oxygenated glass fibers;

[0038] After immersing the surface-modified silica-oxygenated glass fiber in the high-temperature heat-insulating coating, it is dried to obtain modified silica-oxygenated glass fiber.

[0039] On the one hand, it can effectively improve the hydrophobic properties of the prepared modified silica-oxygenated glass fiber, so that the fire suit will not get wet when exposed to water, thereby improving its comfort. On the other hand, it can effectively reduce the thermal conductivity and density of the prepared modified silica-oxygenated glass fiber, thereby significantly improving the thermal insulation performance of the modified silica-oxygenated glass fiber. The prepared modified silica-oxygenated glass fiber improves the thermal resistance of the modified silica-oxygenated glass fiber by inhibiting heat conduction, blocking heat convection, and blocking heat radiation, thereby improving the flame retardant and heat insulation effect of the fire suit.

[0040] It should be noted that, specifically, glass microspheres are a new type of material with wide applications and special properties that has been developed in recent years. They are made from borosilicate raw materials through high-tech processing, with a particle size of 10-250 micrometers and a wall thickness of 1-2 micrometers. They have advantages such as light weight, low thermal conductivity, high strength, and good chemical stability. Their surface is specially treated to have oleophilic and hydrophobic properties, making them very easy to disperse in organic material systems. Silica aerogel can increase the viscosity of coatings and improve their stability.

[0041] In this embodiment, the adhesive solution comprises a high-temperature silicone resin dissolved in cyclohexane. The preferred type of high-temperature silicone resin is silicone resin 908. The selected mass concentration ensures the uniform and stable dissolution of the high-temperature silicone resin in the solvent. Furthermore, the use of this high-temperature silicone resin allows its aryl segments to intercalate between fibers, reducing internal fiber regularity, improving flexibility, and enhancing flame retardancy. At high temperatures, it dehydrates to form layered silica, insulating heat and mass transfer, thus providing a superior flame-retardant effect. Simultaneously, the high-temperature silicone resin used in this application increases the contact angle of the flame-retardant, heat-insulating, and fire-resistant fabric, improving its hydrophobicity.

[0042] In this embodiment, the mass ratio of glass microspheres to silica aerogel is 1:1 to 4:1, for example, 1:1, 1:2, 1:3, 1:4, or any value within this range. By controlling the amount of glass microspheres and silica aerogel added, they work synergistically to create a filler-modified coating with lower density, lower porosity, and lower thermal conductivity. This coating effectively blocks heat transfer through various means, including inhibiting heat conduction, blocking heat convection, and blocking heat radiation, thereby increasing the thermal resistance of the modified silica-oxygenated glass fiber and achieving thermal insulation.

[0043] It should be noted that, specifically, when adding glass microspheres and silica aerogel to the resin solution, the stirring speed is preferably 500-1000 r / min, for example, 500 r / min, 600 r / min, 700 r / min, 800 r / min, 900 r / min, 1000 r / min, or any value within this range; the stirring time is preferably 1.5-3 h, for example, 1.5 h, 2 h, 2.5 h, 3 h, or any value within this range. Controlling the stirring speed and time helps to ensure thorough mixing of the resin solution with the glass microspheres and silica aerogel, resulting in uniform particle distribution in the solution, thus providing a foundation for obtaining high-performance modified silica-oxygenated glass fibers in the subsequent impregnation process.

[0044] In this embodiment, the drying temperature is preferably 100-120℃, such as 100℃, 110℃, 120℃, or any temperature within this range; the drying time is preferably 1-2 minutes, such as 1 minute, 1.5 minutes, 2 minutes, or any time within this range. By controlling the temperature and time of the drying process, a robust and uniform heat-insulating film can be formed on the surface of the silicone-oxygenated glass fiber by the high-temperature heat-insulating coating, thereby improving the flame-retardant and heat-insulating performance of the modified silicone-oxygenated glass fiber.

[0045] Secondly, embodiments of this application also provide modified silica-oxygenated glass fibers prepared by the method described in the first aspect. These modified silica-oxygenated glass fibers possess excellent flame-retardant and thermal insulation properties, hydrophobicity, and comfort.

[0046] Thirdly, embodiments of this application also provide the application of the modified silica-oxygenated glass fiber described in the second aspect in the preparation of flame-retardant, heat-insulating, and fire-resistant fabrics. Based on the excellent flame-retardant, heat-insulating, hydrophobic, and comfortable properties of the modified silica-oxygenated glass fiber, it has wide applications in flame-retardant, heat-insulating, and fire-resistant fabrics.

[0047] Fourthly, embodiments of this application also provide a method for preparing the flame-retardant, heat-insulating, and fire-resistant fabric described in the third aspect. The method includes: using aramid fibers as warp threads for heddling, odd-numbered wefts as aramid fibers, and even-numbered wefts as modified silica-oxygenated glass fibers, and weaving in a double-layer multi-dimensional weaving manner to obtain the flame-retardant, heat-insulating, and fire-resistant fabric.

[0048] It should be noted that, specifically, aramid fibers are used as warp threads for weaving. These fibers act as a skeleton during the weaving process, giving the fabric excellent mechanical properties and high-temperature resistance. Modified silica-based glass fibers are used as even-numbered weft threads. These fibers are located in the sandwich position wrapped by aramid fibers. Double weaving is a special fabric structure. It forms a tight sandwich fabric structure through the overlapping and interlacing of warp threads, thereby enhancing the fabric's density and heat insulation performance. It also maintains structural stability in high-temperature environments and has excellent flame-retardant properties.

[0049] In this embodiment, the aramid fiber includes one or a combination of aramid 1314 fiber and aramid 1414 fiber. Among them, aramid 1313 fiber (meta-aramid) and aramid 1414 fiber (para-aramid) are important high-tech synthetic fibers. They possess excellent high-temperature resistance, flame retardancy, and heat insulation properties, maintaining good physical properties even under high-temperature conditions.

[0050] Fifthly, embodiments of this application also provide a flame-retardant, heat-insulating, and fire-resistant fabric prepared by the method for preparing the flame-retardant, heat-insulating, and fire-resistant fabric described in the fourth aspect, which has a sandwich structure, comprising an aramid fiber as the upper surface layer and a lower surface layer disposed between the modified silica-oxygenated glass fiber of claim 6.

[0051] On the one hand, due to the amide groups in the benzene rings of aramid fibers, the macromolecular chains exhibit a flexible structure and stable chemical structure. When it decomposes under heat, the surface fibers carbonize, continuously blocking heat and slowing down the carbonization rate of the fibers, thus exerting a significant heat-resistant effect. On the other hand, due to its sandwich structure of aramid fibers as the outer layer and modified silica-oxygenated glass fibers as the inner layer, the modified silica-oxygenated glass fibers are located in the interlayer position wrapped by aramid fibers, giving the flame-retardant and heat-insulating fireproof fabric excellent stability. Furthermore, the flame-retardant and heat-insulating fireproof fabric prepared in this application has a minimum thermal conductivity of only 0.0431 mW / m². -1 K -1 It has excellent thermal insulation properties.

[0052] Sixthly, embodiments of this application also provide the application of the flame-retardant, heat-insulating, and fire-resistant fabric described in the fifth aspect in fire-fighting clothing. The excellent flame-retardant, heat-insulating, and fire-resistant properties, hydrophobic and breathable properties, and comfort of the aforementioned flame-retardant, heat-insulating, and fire-resistant fabric enhance the wearer's comfort and work efficiency when used in fire-fighting clothing.

[0053] The technical solution of this application will be further described below with reference to specific embodiments.

[0054] Example 1

[0055] This embodiment provides a method for preparing Al-modified silica-oxygenated glass fibers, specifically including:

[0056] S101: Add 8g of organosilicon resin 908 to 80g of cyclohexane, dissolve at 80℃, and stir at 1000r / min for 1.5h to obtain a resin solution;

[0057] S102: Add 4g of glass microspheres and 1g of silica aerogel to the resin solution and stir at 500r / min for 3h to obtain a high-temperature heat insulation coating.

[0058] S103: The silica-oxygenated glass fiber is impregnated in a 20wt% sodium hydroxide solution and then dried at 80℃.

[0059] S104: The coated fiber is dried in a drying tube at 100°C for 1 minute to obtain Al-modified silica-oxygenated glass fiber.

[0060] Example 2

[0061] This embodiment provides a method for preparing A1-flame-retardant, heat-insulating, and fire-resistant fabric, specifically including:

[0062] Aramid fibers and modified silica-oxygenated glass fibers are woven in a double-layer multi-dimensional process using a weaving machine to obtain A1-flame-retardant, heat-insulating, and fire-resistant fabric.

[0063] Example 3

[0064] This embodiment provides a method for preparing A2-modified silica-oxygenated glass fibers, specifically including:

[0065] S301: Add 8g of organosilicon resin 908 to 80g of cyclohexane, dissolve at 80℃, and stir at 1000r / min for 1.5h to obtain a resin solution;

[0066] S302: 4.8g of glass microspheres and 1.2g of silica aerogel were added, with the amount of glass microspheres being 5% of the mass of cyclohexane. The mixture was stirred at 800r / min for 3h to obtain a high-temperature heat insulation coating.

[0067] S303: Silicone-based glass fibers are impregnated in a 20wt% sodium hydroxide solution and then dried at 80℃.

[0068] S304: The coated fiber is dried in a drying tube at 100°C for 1 minute to obtain A2-modified silica-oxygenated glass fiber.

[0069] Example 4

[0070] This embodiment provides a method for preparing A2-flame-retardant, heat-insulating, and fire-resistant fabric, specifically including:

[0071] Aramid fibers and modified silica-oxygenated glass fibers are woven in a double-layer multi-dimensional process using a weaving machine to obtain A2-flame-retardant, heat-insulating, and fire-resistant fabric.

[0072] Example 5

[0073] This embodiment provides a method for preparing A3-modified silica-oxygenated glass fibers, specifically including:

[0074] S501: Add 8g of organosilicon resin 908 to 80g of cyclohexane, dissolve at 80℃, and stir at 1000r / min for 1.5h to obtain a resin solution;

[0075] S502: Add 5.6g of glass microspheres and 1.4g of silica aerogel to the resin solution and stir at 1000r / min for 2h to obtain a high-temperature heat insulation coating.

[0076] S503: The silica-oxygenated glass fiber is impregnated in a 20wt% sodium hydroxide solution and then dried at 80℃.

[0077] S504: The coated fiber is dried in a drying tube at 120°C for 1 minute to obtain A3-modified silica-oxygenated glass fiber.

[0078] Example 6

[0079] This embodiment provides a method for preparing A3-flame-retardant, heat-insulating, and fire-resistant fabric, specifically including:

[0080] Aramid fibers and modified silica-oxygenated glass fibers are woven in a double-layer multi-dimensional process using a weaving machine to obtain A3-flame-retardant, heat-insulating, and fireproof fabric.

[0081] Example 7

[0082] This embodiment provides a method for preparing A4-modified silica-oxygenated glass fibers, specifically including:

[0083] S701: Add 8g of organosilicon resin 908 to 80g of cyclohexane, dissolve at 80℃, and stir at 1000r / min for 1.5h to obtain a resin solution;

[0084] S702: Add 6.4g of glass microspheres and 1.6g of silica aerogel to the resin solution and stir at 1000r / min for 2h to obtain a high-temperature heat insulation coating.

[0085] S703: The silica-oxygenated glass fiber is impregnated in a 20wt% sodium hydroxide solution and then dried at 80℃.

[0086] S704: The coated fiber is dried in a drying tube at 120°C for 1 minute to obtain A4-modified silica-oxygenated glass fiber.

[0087] Example 8

[0088] This embodiment provides a method for preparing A4 flame-retardant, heat-insulating, and fire-resistant fabric, specifically including:

[0089] Aramid fibers and modified silica-oxygenated glass fibers are woven in a double-layer multi-dimensional process using a weaving machine to obtain A4-flame-retardant, heat-insulating, and fireproof fabric.

[0090] Example 9

[0091] This embodiment provides a method for preparing A5-modified silica-oxygenated glass fibers, specifically including:

[0092] S901: Add 16g of organosilicon resin 908 to 80g of cyclohexane, dissolve at 80℃, and stir at 1000r / min for 1.5h to obtain a resin solution;

[0093] S902: Add 6.4g of glass microspheres and 1.6g of silica aerogel to the resin solution and stir at 500r / min for 3h to obtain a high-temperature heat insulation coating.

[0094] S903: The silica-based glass fiber is impregnated in a 20wt% sodium hydroxide solution and then dried at 80℃.

[0095] S904: The coated fiber is dried in a drying tube at 120°C for 1 minute to obtain A5-modified silica-oxygenated glass fiber.

[0096] Example 10

[0097] This embodiment provides a method for preparing A5-flame-retardant, heat-insulating, and fire-resistant fabric, specifically including:

[0098] Aramid fibers and modified silica-oxygenated glass fibers are woven in a double-layer multi-dimensional process using a weaving machine to obtain A5-flame-retardant, heat-insulating, and fireproof fabric.

[0099] The difference between Embodiment 10 and Embodiment 8 of this application lies in the effect of different adhesive addition amounts on flame-retardant, heat-insulating, and fireproof fabrics.

[0100] Meanwhile, to verify the comprehensive performance of the flame-retardant, heat-insulating, and fireproof fabrics prepared in the above embodiments, this application provides the following comparative examples for detailed illustration.

[0101] Comparative Example 1

[0102] This comparative example provides a method for preparing B1-fabric, specifically including:

[0103] Aramid fibers and glass fibers are woven in a double-layer multidimensional process using a weaving machine to obtain B1-fabric.

[0104] Comparative Example 2

[0105] This comparative example provides a method for preparing B2-fabric, specifically including:

[0106] Aramid fibers are woven using a weaving machine to obtain B2-fabric.

[0107] Comparative Example 3

[0108] This comparative example provides a method for preparing B3-fabric, specifically including:

[0109] S1001: Add 8g of organosilicon resin 908 to 80g of cyclohexane, dissolve at 80℃, and stir at 1000r / min for 1.5h to obtain a resin solution;

[0110] S1002: Add 6.4g of glass microspheres to the resin solution and stir at 1000r / min for 2h to obtain a high-temperature heat insulation coating;

[0111] S1003: Silicone-based glass fibers are impregnated in a 20wt% sodium hydroxide solution and then dried at 80℃.

[0112] S1004: The coated fiber is dried in a drying tube at 100°C for 1 minute to obtain B3-modified silica-oxygenated glass fiber.

[0113] S1005: Aramid fiber and modified silica-oxygenated glass fiber are woven in a double-layer multidimensional process using a weaving machine to obtain B3-fabric.

[0114] Comparative Example 4

[0115] This comparative example provides a method for preparing B4-fabric, specifically including:

[0116] S1101: Add 8g of organosilicon resin 908 to 80g of cyclohexane, dissolve at 80℃, and stir at 1000r / min for 1.5h to obtain a resin solution;

[0117] S1102: Add 1.6g of silica aerogel to the resin solution and stir at 1000r / min for 2h to obtain a high-temperature heat insulation coating;

[0118] S1103: Silicone-based glass fibers are impregnated in a 20wt% sodium hydroxide solution and then dried at 80℃.

[0119] S1104: The coated fiber is dried in a drying tube at 100°C for 1 minute to obtain B4-modified silica-oxygenated glass fiber.

[0120] S1105: Aramid fiber and modified silica-oxygenated glass fiber are woven in a double-layer multidimensional process using a weaving machine to obtain B4-fabric.

[0121] This application presents performance tests on the A1-A4 flame-retardant and heat-insulating fireproof fabrics prepared in the examples and the B1-B4 fabrics prepared in the comparative examples. The test results are shown in Table 1, and the test methods are as follows: Contact angle test: tested using the Finnish Biolin Theta method; Thermal conductivity: tested using the method of GB / T 10295-2008; Microstructure: characterized using a SU8010 scanning electron microscope; Maximum thermal decomposition temperature: tested using a Mettler thermogravimetric analyzer (TGA).

[0122] Table 1. Performance test results of the examples and comparative examples.

[0123]

[0124] As shown in Table 1, thermal conductivity is an important parameter characterizing the heat conduction ability of fabrics; the lower the thermal conductivity, the better the heat insulation effect. Contact angle is the angle formed at the interface between the liquid, solid, and gas phases when a liquid cannot spread on a solid surface and remains in a certain shape. A smaller contact angle indicates better wetting performance, while a larger contact angle makes wetting more difficult. If the contact angle is greater than 90°, the fabric surface cannot be wetted, and the liquid droplets will form beads on the solid surface.

[0125] The performance test results of the A1-A4 flame-retardant and heat-insulating fireproof fabrics prepared according to the embodiments are shown in Table 1. The amount of glass microspheres added varies within the range of this application. All A1-A4 flame-retardant and heat-insulating fireproof fabrics exhibit low thermal conductivity and large contact angles. With the increase of glass microsphere addition, the thermal conductivity of the fabric decreases, while the air permeability, moisture permeability, heat insulation effect, and hydrophobic properties of the fabric are further improved, indicating that all A1-A4 flame-retardant and heat-insulating fireproof fabrics have excellent heat insulation effect and hydrophobic properties. That is, when the glass microsphere addition is in the range of 5-8 wt%, the fabric has good heat insulation effect and good hydrophobic properties, and does not shed powder. The A4 flame-retardant and heat-insulating fireproof fabric has a glass microsphere addition of 8 wt% and a thermal conductivity of 0.0431 mW / m². -1 K -1 With a contact angle of 131°, it boasts the best overall performance.

[0126] The difference between Comparative Example 1 and Example 7 in this application is that the B1-fabric prepared without modification treatment with glass microspheres and silica aerogel has a thermal conductivity of 0.1887 mW / m. -1 K -1Furthermore, its thermal insulation effect is significantly lower than that of A1-A4 flame-retardant and heat-insulating fireproof fabrics. The difference between Comparative Example 2 and Example 7 of this application is that only aramid fibers are used for double-layer multi-dimensional weaving using a weaving machine to obtain pure aramid B2-fabric, which has a thermal conductivity of 0.1710 mW / m². -1 K -1 Furthermore, its thermal insulation effect is significantly lower than that of A1-A4 flame-retardant and heat-insulating fireproof fabrics. The difference between Comparative Example 3 and Example 7 is that the B3-fabric prepared without glass microsphere modification treatment has a thermal conductivity of 0.0598 mW / m². -1 K -1 Furthermore, its thermal insulation effect is significantly lower than that of A1-A4 flame-retardant and heat-insulating fireproof fabrics. The difference between Comparative Example 4 and Example 7 is that the B4-fabric prepared without silica aerogel modification treatment has a thermal conductivity of 0.0987 mW / m³. -1 K -1 Furthermore, its heat insulation effect is significantly lower than that of A1-A4 flame-retardant, heat-insulating, and fireproof fabrics.

[0127] Table 2 Performance test results of fabrics prepared with different adhesive addition amounts

[0128] A4 10％ <![CDATA[0.0431mWm -1 K -1 ]]> 131° No powder loss A6 20％ <![CDATA[0.0435mWm -1 K -1 ]]> 144° No powder loss

[0129] To verify the preparation mechanism diagram of the flame-retardant, heat-insulating, and fire-resistant fabric prepared in the embodiments of this application, the results are as follows: Figures 1 to 2 As shown. Among them, Figure 1 A diagram showing the woven structure of a flame-retardant, heat-insulating, and fire-resistant fabric. Figure 2 This is a schematic diagram of the process for Al-modified silica-oxygenated glass fiber.

[0130] according to Figure 1 As is known, a) is the weaving diagram, indicating that every 4 fibers are inserted into one reed; b) is the fiber structure diagram of the fabric; and c) is the machine program diagram of the semi-automatic sample making machine. The fabric is woven by two systems of warp yarns (i.e., outer warp and inner warp) and one system of weft yarns through double multidimensional weaving, and finally forms a sandwich structure with aramid fiber as the outer layer and modified silicone oxygen glass fiber as the inner layer.

[0131] according to Figure 2 As is known, glass fibers are first surface-treated with sodium hydroxide to remove surface impurities, and then introduced into a high-temperature thermally conductive coating to composite glass microspheres and silica aerogel into the interior of the silica-oxygenated glass fibers. After further drying, modified silica-oxygenated glass fibers are obtained.

[0132] To verify the morphology and structure of the flame-retardant, heat-insulating, and fire-resistant fabric prepared in the embodiments of this application, the results are as follows: Figures 3 to 5 As shown. Among them, Figure 3 Scanning electron microscope image of Al-modified silica-oxygenated glass fiber; Figure 4A scanning electron microscope image of a planar surface of A1-flame-retardant, heat-insulating, and fire-resistant fabric; Figure 5 Scanning electron microscope image of a cross section of A1-flame-retardant, heat-insulating, and fireproof fabric.

[0133] according to Figure 3 As can be seen from the scanning electron microscope images of the modified silica-oxygenated glass fibers, glass microspheres are clearly uniformly loaded into the fiber interior.

[0134] according to Figure 4 and Figure 5 As is known, after multidimensional weaving of aramid fibers and glass microspheres loaded with silica-oxygenated glass fibers, a temperature gradient double fabric with a flame-retardant and fire-resistant layer and a thermal insulation layer is obtained. The glass microspheres loaded with silica-oxygenated glass fibers in the thermal insulation interlayer form a closed-cell spherical micro-nano structure, which is not only hydrophobic but also thermally insulating. The upper and lower surfaces are made of flame-retardant and fire-resistant aramid fibers, which gives the fabric both flame-retardant and fire-resistant and heat-insulating functions.

[0135] To verify the comprehensive performance of the flame-retardant and heat-insulating fabric prepared in the embodiments of this application, the results are as follows: Figure 6 As shown. Among them, Figure 6 This is the DTG diagram for A1-flame-retardant, heat-insulating, and fire-resistant fabric.

[0136] according to Figure 6 It can be seen that as the amount of glass microspheres added increases, the maximum thermal decomposition temperature gradually increases, and the thermal stability gradually increases.

[0137] Therefore, the preparation method provided in this application obtains high-temperature heat-insulating coating modified silica-oxygenated glass fiber by using glass microspheres, silica aerogel and resin solution, and uses aramid fiber as warp yarn for heddling, with odd-numbered wefts being aramid fiber and even-numbered wefts being modified silica-oxygenated glass fiber. It is woven in a double multi-dimensional weaving manner to obtain flame-retardant heat-insulating fireproof fabric. It is made into a sandwich structure with aramid fiber as the upper and lower surface layer and modified silica-oxygenated glass fiber as the inner layer. Due to its excellent heat insulation and fireproof performance, it has a wide application in fire-fighting clothing.

[0138] The various embodiments in this specification are described in a progressive manner. The same or similar parts between the various embodiments can be referred to each other. Each embodiment focuses on describing the differences from other embodiments.

[0139] The above embodiments are only used to illustrate the technical solutions of this application, and are not intended to limit this application. Although this application has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of this application.

Claims

1. A method for preparing modified silica-oxygenated glass fiber, characterized in that, The method includes: Glass microspheres and silica aerogel are added to an adhesive solution of 5-20 wt% to obtain a high-temperature heat-insulating coating. Silicon-oxygenated glass fibers are immersed in an alkaline solution for treatment to obtain surface-modified silicon-oxygenated glass fibers; After immersing the surface-modified silica-oxygenated glass fiber in the high-temperature heat-insulating coating, it is dried to obtain modified silica-oxygenated glass fiber. The adhesive solution includes a high-temperature organosilicon resin dissolved in cyclohexane; The mass ratio of the glass microspheres to the silica aerogel is 1:1 to 4:1; The drying process is carried out at a temperature of 100-120℃ for 1-2 minutes.

2. A modified silica-oxygenated glass fiber prepared by the method of preparation of the modified silica-oxygenated glass fiber according to claim 1.

3. The application of the modified silica-oxygenated glass fiber according to claim 2 in the preparation of flame-retardant, heat-insulating, and fire-resistant fabrics.

4. A method for preparing a flame-retardant, heat-insulating, and fire-resistant fabric, characterized in that, The method includes: using aramid fiber as the warp for heddling, odd-numbered wefts being aramid fiber, and even-numbered wefts being the modified silica-oxygenated glass fiber as described in claim 2, and weaving in a double-layer multi-dimensional weaving manner to obtain a flame-retardant, heat-insulating, and fireproof fabric.

5. The method for preparing flame-retardant, heat-insulating, and fire-resistant fabric according to claim 4, characterized in that, The aramid fiber includes one or a combination of aramid 1314 fiber and aramid 1414 fiber.

6. A flame-retardant, heat-insulating, and fire-resistant fabric prepared by the method according to any one of claims 4-5, having a sandwich structure, characterized in that, Includes the modified silica-oxygenated glass fiber of claim 2, which has an aramid fiber as the upper and lower surface layer and is disposed therebetween.

7. The application of the flame-retardant, heat-insulating, and fire-resistant fabric according to claim 6 in the manufacture of fire-fighting suits.

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