A ceramicized silicone-based multilayer fibrous fireproof cloth and a preparation method thereof

Abstract

The present application relates to a kind of ceramic organic silicon-based multilayer fiber fireproof cloth and its preparation method.The multilayer fiber fireproof cloth includes flexible base layer and high-temperature-resistant layer attached to both sides of flexible base layer;The flexible base layer is the flexible base layer of ceramic organic silicon layer-inorganic fiber cloth layer-ceramic organic silicon layer-inorganic fiber cloth layer-ceramic organic silicon layer superposition;The high-temperature-resistant layer is high-silicon cloth;The ceramic organic silicon layer has closed-cell foam pore.The flexible base layer of multilayer fiber fireproof cloth is foamed by using step-by-step heating vulcanization, with good closed cell;Flexible base layer dispersed ceramic short fiber, fluxing agent, not only improve the strength of fireproof cloth, and high-temperature ceramic after maintaining the mechanical properties and dimensional stability of ceramic layer, support pore is not easy to collapse, prevent ceramic layer cracking, effectively insulate heat transfer when high-temperature thermal shock, prevent fire spread.The present application uses liquid silicone rubber, easy to process, realize automatic continuous production.

Description

Technical Field

[0001] This invention relates to the field of layered fireproof fabric made of fibers, and specifically to a multilayer fiber fireproof fabric based on ceramicized organosilicon and its preparation method. Background Technology

[0002] Inorganic fiber cloth, due to its good high-temperature resistance and fire resistance, can effectively slow down heat transfer when used as fireproof cloth. However, when used for fire extinguishing and heat insulation, air easily permeates the inorganic fiber cloth, reducing its oxygen-barrier and flame-retardant properties, making it difficult to fundamentally block heat transfer. In scenarios such as welding operations, chemical reactions, high-temperature pipelines, and fires in new energy vehicles, it is required to quickly block the spread of the fire source and curb heat transfer in the early stages of a fire, buying time for fire rescue and surrounding safety. Therefore, there are high requirements for fireproof cloth in terms of isolating air and blocking heat transfer.

[0003] Fireproof cloth obtained by coating glass fiber cloth with ceramicized silicone rubber not only increases the air isolation effect, but also transforms the ceramicized silicone rubber into a hard ceramic-like shell at high temperatures. This shell not only provides heat insulation but can also withstand thermal shock exceeding 1000℃, showing great potential for application in high-performance fireproof cloth. Currently, most high-performance fireproof cloths use ceramicized silicone rubber coated with inorganic fiber cloth. Chinese patent CN115674828B discloses a multi-layer fireproof material for batteries and its preparation method, including a fireproof material substrate and a protective layer covering the outer surface of the fireproof material substrate; the fireproof material substrate, from top to bottom, includes a first glass fiber cloth layer, a ceramicized silicone rubber layer, and a second glass fiber cloth layer; it has good flame-retardant and fire-resistant effects and high-temperature flame impact resistance. Chinese patent CN117507515B discloses a high-temperature ceramicizable fireproof and heat-insulating pad with an inorganic fiber cloth as the skeleton, using woven inorganic fiber cloth as the skeleton material and silicone rubber elastic ceramicizable composite material, which can resist the high-intensity thermal jets during battery cell eruption.

[0004] The aforementioned composite of ceramicized silicone rubber and fiberglass cloth has achieved certain effects in isolating air penetration and resisting thermal shock, forming a ceramicized protective layer with a flame retardant rating of UL94 V-0. However, its use as fireproof cloth still has shortcomings in blocking heat transfer. This is mainly because the ceramicized silicone rubber often shrinks and deforms after high-temperature ceramicization, leading to cracking of the ceramic layer or collapse of micropores, preventing the formation of a continuous ceramic body. This weakens the heat insulation effect under thermal shock and affects its ability to prevent heat spread. Summary of the Invention

[0005] To address the problem that ceramicized silicone rubber composite fiber cloth is prone to cracking after ceramicization, affecting its heat insulation, this invention proposes a multi-layer fiber fireproof cloth based on ceramicized organosilicon. By designing a ceramicized organosilicon layer with closed-cell foam pores between the fireproof cloth layers, it combines air barrier, heat insulation, and flexibility.

[0006] The specific solution to achieve the above technical objectives is as follows:

[0007] In a first aspect, the present invention provides a multilayer fiber fireproof cloth based on ceramicized organosilicon, comprising a flexible base layer and high-temperature resistant layers adhered to both sides of the flexible base layer; the flexible base layer is a flexible base layer composed of ceramicized organosilicon layer - inorganic fiber cloth layer - ceramicized organosilicon layer - inorganic fiber cloth layer - ceramicized organosilicon layer; the high-temperature resistant layer is a high-silica cloth.

[0008] The ceramicized organosilicon layer has closed-cell foam pores;

[0009] The inorganic fiber cloth layer is at least one of glass fiber cloth and ceramic fiber cloth;

[0010] The high-silica fabric is a satin-woven high-silica fiber fabric with a silica content of ≥96%.

[0011] Furthermore, the ceramicized organosilicon layer is obtained by addition vulcanization of the following raw materials in parts by weight: 100 parts vinyl silicone oil, 4-6 parts hydroxyl silicone oil, 40-50 parts ceramicized filler, 10-15 parts aluminum hydroxide, 5-10 parts ceramic short fibers, 3-5 parts fumed silica, 3-5 parts flux, 8-10 parts hydrogen-containing silicone oil, 0.3-0.5 parts platinum catalyst, and 0.1-0.2 parts inhibitor; the ceramicized filler is composed of one or more of low-melting-point glass powder, alumina powder, mica powder, kaolin, and silica powder in a mass ratio of 3:(2-3); the flux is composed of calcium carbonate, potassium fluorosilicate, and borax in a mass ratio of 2:(1-2).

[0012] Furthermore, the thickness of the ceramicized silicone layer is 0.5–1.0 mm. The ceramicized silicone layer has good closed-cell foam pores, exhibiting excellent elasticity, giving the fireproof cloth flexibility, and allowing the folded fireproof cloth to be easily and quickly unfolded for convenient use.

[0013] Furthermore, the softening point temperature of the low melting point glass powder is 600–800°C.

[0014] Furthermore, the ceramic short fibers are at least one of alumina fibers, mullite fibers, aluminosilicate fibers, and zirconium oxide fibers. By using ceramic short fibers in the ceramicized organosilicon layer, excellent dimensional stability is exhibited during high-temperature ceramicization and subsequent rapid temperature increases. This maintains the relative stability of the closed-cell ceramic body volume, achieving structural integrity and thermal insulation under high-temperature flame impact.

[0015] Furthermore, the inorganic fiber cloth layer is a plain-weave inorganic fiber cloth with a thickness of 0.2 to 0.5 mm.

[0016] Furthermore, the high-silica fabric is a satin-woven high-silica fiber fabric with a thickness of 0.4 to 1.3 mm.

[0017] Furthermore, the hydroxyl silicone oil is a medium-hydroxyl-value hydroxyl silicone oil with a hydroxyl content of 4-6% by mass. In the ceramicized organosilicon layer, vinyl silicone oil serves as the base material. Under the action of a platinum catalyst, it undergoes an addition reaction with hydrogen-containing silicone oil containing silicon-hydrogen bonds (Si–H) to generate silicone rubber. Simultaneously, the hydrogen-containing silicone oil containing silicon-hydrogen bonds (Si–H) undergoes a condensation dehydrogenation reaction with the hydroxyl groups (-OH) of the hydroxyl silicone oil, stably generating hydrogen gas for in-situ foaming, thereby obtaining closed-cell foam pores.

[0018] Furthermore, the platinum catalyst is a Castells platinum catalyst with a platinum concentration of 500 ppm.

[0019] Furthermore, the inhibitor is an alkynyl alcohol inhibitor, specifically at least one of 1-ethynyl-1-cyclohexanol and 3,7,11-trimethyldodecyn-3-ol. The inhibitor prevents premature crosslinking of the vinyl silicone oil during mixing and coating, prevents excessively rapid reaction during heating, and promotes the formation of a uniform closed-cell structure during subsequent stepwise heating and crosslinking vulcanization.

[0020] Secondly, the present invention provides a method for preparing a multilayer fiber fireproof cloth based on ceramicized organosilicon, comprising the following steps:

[0021] (1) Add 100 parts of vinyl silicone oil, 4-6 parts of hydroxyl silicone oil, 40-50 parts of ceramicized filler, 10-15 parts of aluminum hydroxide, 5-10 parts of ceramic short fibers, 3-5 parts of fumed silica, and 3-5 parts of flux to a three-roll mill for grinding and dispersion to obtain a first-stage material; add 8-10 parts of hydrogen-containing silicone oil, 0.3-0.5 parts of platinum catalyst, and 0.1-0.2 parts of inhibitor to a three-roll mill for grinding and dispersion to obtain a second-stage material;

[0022] (2) The first and second materials are mixed evenly in a planetary mixer to form a ceramicized organosilicon material, which is then coated on the front and back of the inorganic fiber cloth. The two layers are then stacked to form a layered structure of ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer. High-silica cloth is bonded to the ceramicized organosilicon layers on both sides. The cloth is shaped by a calender and vulcanized in a tunnel furnace in stages. The vulcanization zone temperatures are 80℃ for primary vulcanization foaming, 100℃ for secondary vulcanization foaming, 120℃ for tertiary vulcanization foaming, and 140℃ for quaternary vulcanization. The cloth is cooled and shaped by a shaping roller and then wound up to obtain a multi-layer fiber fireproof cloth based on ceramicized organosilicon.

[0023] Understandably, the closed-cell structure of the ceramicized silicone layer, after ceramic formation, results in extremely low thermal conductivity, effectively blocking heat transfer and preventing the penetration of flames and high-temperature gases. However, the problem is that when the ceramicized silicone layer encounters high temperatures and undergoes ceramicization, shrinkage and cell collapse prevent the ceramicized protective layer from forming a complete barrier, thus affecting the heat insulation effect and limiting its ability to prevent heat spread.

[0024] This invention discloses a multi-layer fiber fireproof cloth based on ceramicized organosilicon. Addressing the aforementioned issues, it utilizes a hydroxyl silicone oil with a moderate hydroxyl value to achieve stable condensation of hydrogen-containing silicone oil and hydroxyl silicone oil, generating hydrogen gas for in-situ foaming. The gas generation rate is controlled, and the cloth is vulcanized in a tunnel furnace with progressively increasing temperatures. The cross-linked vulcanized silicone rubber forms closed-cell structures. Ceramic short fibers and flux are used in the ceramicized organosilicon layer. When used for fireproofing, as the high temperature gradually reaches the internal flexible base layer of the ceramicized organosilicon layer, the ceramicized filler gradually ceramicizes above 600°C. The flux promotes uniform melting of the ceramic melt. Above 800°C, calcium carbonate gradually generates CO2 gas, which is sealed in situ by the melt, forming a closed-cell structure. This ensures the integrity of the closed-cell structure of the ceramicized layer and provides continuous thermal insulation performance. Furthermore, the ceramic short fibers are integrated with the ceramic, exhibiting excellent high-temperature dimensional stability and strength, preventing the ceramic layer from cracking under high-temperature flame impact.

[0025] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0026] (1) The flexible base layer of the multi-layer fiber fireproof cloth is vulcanized and foamed by step-by-step heating to form a silicone rubber layer with good closed-cell foam. At high temperature, it is transformed into a closed-cell self-supporting ceramic protective layer. By promoting melting and sintering, the ceramic layer forms a high-hardness ceramic body on the basis of closed-cell foam, which effectively isolates heat transfer and oxygen permeation, and plays a good flame-retardant role, preventing the spread of fire.

[0027] (2) The flexible base layer of the multilayer fiber fireproof cloth is dispersed with short ceramic fibers, which not only improves the strength of the fireproof cloth, but also maintains the mechanical properties and dimensional stability of the ceramic layer after high-temperature ceramicization. The flux promotes the formation of closed pores in the melt during ceramicization, supports the pores to prevent collapse, prevents the ceramic layer from cracking, and prevents heat transfer during high-temperature thermal shock.

[0028] (3) Multi-layer fiber fireproof cloth is flexible and easy to fold and carry. The outermost layer is a high-silica cloth layer that is resistant to high temperature and directly contacts the fire source. It can withstand high temperatures above 1000℃ and can quickly cover the initial flame. Later, it forms a ceramic layer that is heat-insulating and oxygen-barrier. It is resistant to the thermal shock of high-temperature flames and is suitable for covering the fire source in scenarios such as welding slag fire, chemical reaction raw material fire, and lithium battery fire, restricting air entry and blocking the fire source from spreading outward.

[0029] (4) The present invention uses liquid silicone rubber, which is easy to process and mold, realizes automated continuous production, and has a short production cycle and high efficiency. Attached Figure Description

[0030] Figure 1 This is a schematic diagram of a multilayer fiber fireproof cloth based on ceramicized organosilicon according to the present invention, wherein: 1 is a flexible base layer; 101 is a ceramicized organosilicon layer; 102 is an inorganic fiber cloth layer; and 2 is a high-temperature resistant layer.

[0031] Figure 2 This is a partial view of the ceramicized organosilicon layer of the multilayer fiber fireproof cloth in Example 1.

[0032] Figure 3 This is a partial view of the ceramicized organosilicon layer of the multilayer fiber fireproof cloth in Example 1 after ablation and ceramicization.

[0033] Figure 4 This is a partial view of the ceramicized organosilicon layer of the multi-layer fiber fireproof cloth in Comparative Example 1 after ablation and ceramicization.

[0034] Figure 5 It is a graph showing the temperature-time change of the unexposed side of the fireproof cloth during ablation. Detailed Implementation

[0035] To enable those skilled in the art to better understand the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are merely some embodiments of the present invention and are not intended to limit the scope of this application. Based on the embodiments of the present invention, simple substitutions made by those skilled in the art without creative effort should fall within the scope of protection of the present invention.

[0036] In the specific implementation scheme described below, the inorganic fiber cloth used has a thickness of 0.3 mm and a plain weave density of 100 g / m². 2 The ceramic fiber cloth (alumina content greater than 90%) is used; the high silica cloth used is a 0.65mm thick, satin-woven high silica fiber cloth (silica content greater than 96%).

[0037] Some of the materials used in this application:

[0038] Vinyl silicone oil: Vinyl-terminated polydimethylsiloxane, brand name ADL, viscosity approximately 2000 mPa·s, provided by Jiangxi Andeli High-Tech Technology Co., Ltd.

[0039] Hydrogen-containing silicone oil: RH202-20, hydrogen content 1.55%, Zhejiang Runhe Organosilicon New Materials Co., Ltd.

[0040] Hydroxyl silicone oil: 6% hydroxyl content, Zhejiang Runhe Organosilicon New Materials Co., Ltd.

[0041] Platinum catalyst: Castells platinum catalyst with a platinum concentration of 500 ppm.

[0042] This invention provides a multilayer fiber fireproof cloth based on ceramicized organosilicon, such as... Figure 1 The structure shown is as follows: 1 is a flexible base layer; 101 is a ceramicized silicone layer; 102 is an inorganic fiber cloth layer; and 2 is a high-temperature resistant layer. The flexible base layer is composed of layers of ceramicized silicone, inorganic fiber cloth, ceramicized silicone, inorganic fiber cloth, and ceramicized silicone, with high-temperature resistant layers bonded to both sides of the flexible base layer. The ceramicized silicone layer contains abundant closed-cell foam pores.

[0043] A multilayer fiber fireproof cloth based on ceramicized organosilicon is prepared by the following method:

[0044] (1) Add vinyl silicone oil, hydroxyl silicone oil, ceramicized filler, aluminum hydroxide, ceramic short fiber, fumed silica and flux to a three-roll mill for grinding and dispersion to obtain a first-stage material; add hydrogen-containing silicone oil, platinum catalyst and inhibitor to a three-roll mill for grinding and dispersion to obtain a second-stage material;

[0045] (2) The first and second materials are mixed evenly in a planetary mixer to form a ceramicized organosilicon material, which is then coated on the front and back of the inorganic fiber cloth. The two layers are then stacked to form a layered structure of ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer. High-silica cloth is bonded to the ceramicized organosilicon layers on both sides. The cloth is shaped by a calender and vulcanized by step-by-step temperature increase in a tunnel furnace. The cross-linked vulcanized silicone rubber locks the cells, forming a closed-cell cell structure. The cloth is cooled and shaped by a shaping roller and then wound up to obtain a multi-layer fiber fireproof cloth based on ceramicized organosilicon.

[0046] Example 1

[0047] (1) 100 parts of vinyl silicone oil, 4 parts of hydroxyl silicone oil, 40 parts of ceramicized filler, 10 parts of aluminum hydroxide, 6 parts of aluminum silicate ceramic short fibers (fiber length less than 1 mm), 3 parts of fumed silica (particle size 0.5-1 μm), and 3 parts of flux were added to a three-roll mill for grinding and dispersion to obtain a first-stage material; 8 parts of hydrogen-containing silicone oil, 0.3 parts of platinum catalyst, and 0.2 parts of inhibitor 1-ethynyl-1-cyclohexanol were ground and dispersed in a three-roll mill to obtain a second-stage material; wherein, the ceramicized filler was composed of low melting point glass powder (softening point 650℃) and alumina powder (1250 mesh) in a mass ratio of 3:2; the flux was composed of calcium carbonate and potassium fluorosilicate in a mass ratio of 2:1;

[0048] (2) The first and second materials are mixed evenly in a planetary mixer to form a ceramicized organosilicon material. It is then coated on both sides of the inorganic fiber cloth with a coating thickness of 0.2 mm. The two layers of inorganic fiber cloth are then stacked to form a layered structure of ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer. High-silica cloth is bonded to the ceramicized organosilicon layers on both sides. The cloth is shaped by a calender and then vulcanized by step-by-step heating in a tunnel furnace. The vulcanization is carried out in the first vulcanization zone at 80℃ for 3 min, the second vulcanization zone at 100℃ for 5 min, the third vulcanization zone at 120℃ for 8 min, and the fourth vulcanization zone at 140℃ for 10 min. The cloth is then cooled and shaped by a shaping roller and rolled up to obtain a multi-layer fiber fireproof cloth based on ceramicized organosilicon.

[0049] After vulcanization and foaming, the ceramicized organosilicon layer of the multi-layer fiber fireproof cloth exhibits excellent closed-cell structure. A partial electron microscope image of the cross-section of the ceramicized organosilicon layer after cutting reveals the formation of well-defined closed cells. Figure 2 The ceramicized organosilicon layer was continuously ablated for 5 minutes using an 800℃ flame gun. The ablated and ceramicized organosilicon layer maintained its intact structure, without obvious cracking or structural collapse, and the closed pores remained intact. Figure 3 .

[0050] Example 2

[0051] (1) 100 parts of vinyl silicone oil, 6 parts of hydroxyl silicone oil, 45 parts of ceramicized filler, 15 parts of aluminum hydroxide, 5 parts of mullite short fiber (fiber length less than 1 mm), 5 parts of fumed silica (particle size 0.5-1 μm), and 5 parts of flux were added to a three-roll mill for grinding and dispersion to obtain a first-stage material; 10 parts of hydrogen-containing silicone oil, 0.5 parts of platinum catalyst, and 0.1 parts of inhibitor 3,7,11-trimethyldodecyn-3-ol were ground and dispersed in a three-roll mill to obtain a second-stage material; wherein, the ceramicized filler was composed of low melting point glass powder (softening point 650℃) and kaolin (1250 mesh) in a mass ratio of 3:2.5; the flux was composed of calcium carbonate and potassium fluorosilicate in a mass ratio of 2:1.5.

[0052] (2) The first and second materials are mixed evenly in a planetary mixer to form a ceramicized organosilicon material. It is then coated on both sides of the inorganic fiber cloth with a coating thickness of 0.2 mm. The two layers of inorganic fiber cloth are then stacked to form a layered structure of ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer. High-silica cloth is bonded to the ceramicized organosilicon layers on both sides. The cloth is shaped by a calender and then vulcanized by step-by-step heating in a tunnel furnace. The vulcanization is carried out in the first vulcanization zone at 80℃ for 3 min, the second vulcanization zone at 100℃ for 5 min, the third vulcanization zone at 120℃ for 8 min, and the fourth vulcanization zone at 140℃ for 10 min. The cloth is then cooled and shaped by a shaping roller and rolled up to obtain a multi-layer fiber fireproof cloth based on ceramicized organosilicon.

[0053] Comparative Example 1

[0054] (1) 100 parts of vinyl silicone oil, 4 parts of hydroxyl silicone oil, 40 parts of ceramicized filler, 10 parts of aluminum hydroxide, and 3 parts of fumed silica (particle size 0.5-1μm) were added to a three-roll mill for grinding and dispersion to obtain a first-stage material; 8 parts of hydrogen-containing silicone oil, 0.3 parts of platinum catalyst, and 0.2 parts of inhibitor 1-ethynyl-1-cyclohexanol were ground and dispersed in a three-roll mill to obtain a second-stage material; wherein, the ceramicized filler was composed of low-melting-point glass powder (softening point 650℃) and alumina powder (1250 mesh) in a mass ratio of 3:2;

[0055] (2) The first and second materials are mixed evenly in a planetary mixer to form a ceramicized organosilicon material. It is then coated on both sides of the inorganic fiber cloth with a coating thickness of 0.2 mm. The two layers of inorganic fiber cloth are then stacked to form a layered structure of ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer. High-silica cloth is bonded to the ceramicized organosilicon layers on both sides. The cloth is shaped by a calender and then vulcanized by step-by-step heating in a tunnel furnace. The vulcanization is carried out in the first vulcanization zone at 80℃ for 3 min, the second vulcanization zone at 100℃ for 5 min, the third vulcanization zone at 120℃ for 8 min, and the fourth vulcanization zone at 140℃ for 10 min. The cloth is then cooled and shaped by a shaping roller and rolled up to obtain a multi-layer fiber fireproof cloth based on ceramicized organosilicon.

[0056] After vulcanization and foaming, the ceramicized organosilicon layer of the multi-layer fiber fireproof cloth has good closed-cell structure. However, due to the lack of support from short ceramic fibers and the absence of flux to promote uniform melting of the ceramic melt, the ceramicized organosilicon layer was continuously ablated for 5 minutes using an 800℃ flame gun. After ablation and ceramicization, cracks appeared in the ceramicized organosilicon layer, and some of the cell structure collapsed. Figure 4 .

[0057] Comparative Example 2

[0058] (1) 100 parts of vinyl silicone oil, 4 parts of hydroxyl silicone oil, 40 parts of ceramicized filler, 10 parts of aluminum hydroxide, 6 parts of aluminum silicate ceramic short fibers (fiber length less than 1 mm), 3 parts of fumed silica (particle size 0.5-1 μm), and 3 parts of flux were added to a three-roll mill for grinding and dispersion to obtain a first-stage material; 8 parts of hydrogen-containing silicone oil, 0.3 parts of platinum catalyst, and 0.2 parts of inhibitor 1-ethynyl-1-cyclohexanol were ground and dispersed in a three-roll mill to obtain a second-stage material; wherein, the ceramicized filler was composed of low melting point glass powder (softening point 650℃) and alumina powder (1250 mesh) in a mass ratio of 3:2; the flux was composed of calcium carbonate and potassium fluorosilicate in a mass ratio of 2:1;

[0059] (2) The first and second materials are mixed evenly in a planetary mixer to form a ceramicized organosilicon material. It is then coated on both sides of the inorganic fiber cloth with a coating thickness of 0.2 mm. The two layers of inorganic fiber cloth are then stacked to form a layered structure of ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer. High-silica cloth is bonded to the ceramicized organosilicon layers on both sides. The cloth is then shaped by a calender, vulcanized and foamed at 120°C for 26 min, cooled and shaped by a shaping roller, and then wound up to obtain a multi-layer fiber fireproof cloth based on ceramicized organosilicon.

[0060] Instead of using a stepwise heating foaming method, this scheme uses continuous high-temperature vulcanization foaming at 120℃, which results in more intense foaming and slightly poorer closed-cell performance of the ceramicized organosilicon layer.

[0061] Fire resistance and heat spread prevention performance test:

[0062] The fireproof cloth used in Examples 1-2 and Comparative Examples 1-2 was 4.2 mm thick. One side of the fireproof cloth was ablated using an 800°C flame gun at a distance of 5 cm. The temperature on the other side (the unexposed side) was collected using a thermocouple (initial temperature 27°C). The temperature change of the unexposed side over time during the 10-minute ablation process is recorded (see Table 1). The temperature-time curve of the unexposed side is shown below. Figure 5 .

[0063] Table 1:

[0064]

[0065] By recording the temperature rise on the unexposed side, the fireproof cloth of this invention exhibits excellent closed-cell structure in its middle layer. In the initial stage of ablation (within 5 minutes), the pores in the flexible base layer effectively block the spread of fire, resulting in a slow temperature rise. As the high temperature of the flame gradually propagates to the ceramicized organosilicon layer of the internal flexible base layer, ceramicization occurs, and the temperature on the unexposed side rises to approximately 120°C. Thereafter, the ceramicized layer inhibits the rapid spread of the high-temperature flame. After 10 minutes of ablation, the fireproof cloth showed no cracking, powdering, or layer detachment.

[0066] Comparative Example 1, lacking the support of short ceramic fibers and the flux to promote uniform melting of the ceramic melt, exhibited good thermal insulation in the initial stage of ablation. However, as the temperature increased and ceramization progressed, cracks appeared in the ceramization layer, some of the cell structure collapsed, heat spread was rapid, and the temperature on the unexposed side rose faster. Comparative Example 2 had slightly poorer cell closure, resulting in slightly faster initial temperature transfer. After ceramization in the later stages, the temperature on the unexposed side rose relatively quickly.

Claims

1. A multilayer fiber fireproof cloth based on ceramicized organosilicon, characterized in that, The multi-layer fiber fireproof cloth includes a flexible base layer and high-temperature resistant layers adhered to both sides of the flexible base layer; the flexible base layer is a flexible base layer composed of a ceramicized organosilicon layer, an inorganic fiber cloth layer, a ceramicized organosilicon layer, an inorganic fiber cloth layer, and a ceramicized organosilicon layer; the high-temperature resistant layer is a high-silica cloth. The ceramicized organosilicon layer has closed-cell foam pores; the ceramicized organosilicon layer is obtained by addition vulcanization of the following raw materials in parts by weight: 100 parts vinyl silicone oil, 4-6 parts hydroxyl silicone oil, 40-50 parts ceramicized filler, 10-15 parts aluminum hydroxide, 5-10 parts ceramic short fibers, 3-5 parts fumed silica, 3-5 parts flux, 8-10 parts hydrogen-containing silicone oil, 0.3-0.5 parts platinum catalyst, and 0.1-0.2 parts inhibitor; the hydroxyl silicone oil is a medium-hydroxyl-value hydroxyl silicone oil with a hydroxyl content of 4-6% by mass; the ceramicized filler is composed of one or more of low-melting-point glass powder, alumina powder, mica powder, kaolin, and silica powder in a mass ratio of 3:(2-3); the flux is composed of calcium carbonate, potassium fluorosilicate, and borax in a mass ratio of 2:(1-2). The inorganic fiber cloth layer is at least one of glass fiber cloth and ceramic fiber cloth; The high-silica fabric is a satin-woven high-silica fiber fabric with a silica content of ≥96%; The multilayer fiber fireproof cloth based on ceramicized organosilicon is prepared by the following method: (1) Add 100 parts of vinyl silicone oil, 4-6 parts of hydroxyl silicone oil, 40-50 parts of ceramicized filler, 10-15 parts of aluminum hydroxide, 5-10 parts of ceramic short fibers, 3-5 parts of fumed silica, and 3-5 parts of flux to a three-roll mill for grinding and dispersion to obtain a first-stage material; add 8-10 parts of hydrogen-containing silicone oil, 0.3-0.5 parts of platinum catalyst, and 0.1-0.2 parts of inhibitor to a three-roll mill for grinding and dispersion to obtain a second-stage material; (2) The first and second materials are mixed evenly in a planetary mixer to form a ceramicized organosilicon material, which is then coated on the front and back of the inorganic fiber cloth. The two layers are then stacked to form a layered structure of ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer. High-silica cloth is bonded to the ceramicized organosilicon layers on both sides. The cloth is shaped by a calender and vulcanized in a tunnel furnace in stages. The vulcanization zone temperatures are 80℃ for primary vulcanization foaming, 100℃ for secondary vulcanization foaming, 120℃ for tertiary vulcanization foaming, and 140℃ for quaternary vulcanization. The cloth is cooled and shaped by a shaping roller and then wound up to obtain a multi-layer fiber fireproof cloth based on ceramicized organosilicon.

2. The multilayer fiber fireproof cloth based on ceramicized organosilicon according to claim 1, characterized in that, The thickness of the ceramicized organosilicon layer is 0.5–1.0 mm.

3. The multilayer fiber fireproof cloth based on ceramicized organosilicon according to claim 1, characterized in that, The softening point temperature of the low melting point glass powder is 600-800℃.

4. The multilayer fiber fireproof cloth based on ceramicized organosilicon according to claim 1, characterized in that, The inorganic fiber cloth layer is a plain-weave inorganic fiber cloth with a thickness of 0.2 to 0.5 mm.

5. The multilayer fiber fireproof cloth based on ceramicized organosilicon according to claim 1, characterized in that, The ceramic short fibers are at least one of alumina fibers, mullite fibers, aluminosilicate fibers, and zirconium oxide fibers.

6. The multilayer fiber fireproof cloth based on ceramicized organosilicon according to claim 1, characterized in that, The high-silica fabric is a satin-woven high-silica fiber fabric with a thickness of 0.4 to 1.3 mm.

7. The multilayer fiber fireproof cloth based on ceramicized organosilicon according to claim 1, characterized in that, The inhibitor is at least one of 1-ethynyl-1-cyclohexanol and 3,7,11-trimethyldodecyn-3-ol.

8. The method for preparing the multilayer fiber fireproof cloth based on ceramicized organosilicon as described in any one of claims 1 to 7, characterized in that, Includes the following steps: (1) Add 100 parts of vinyl silicone oil, 4-6 parts of hydroxyl silicone oil, 40-50 parts of ceramicized filler, 10-15 parts of aluminum hydroxide, 5-10 parts of ceramic short fibers, 3-5 parts of fumed silica, and 3-5 parts of flux to a three-roll mill for grinding and dispersion to obtain a first-stage material; add 8-10 parts of hydrogen-containing silicone oil, 0.3-0.5 parts of platinum catalyst, and 0.1-0.2 parts of inhibitor to a three-roll mill for grinding and dispersion to obtain a second-stage material; (2) The first and second materials are mixed evenly in a planetary mixer to form a ceramicized organosilicon material, which is then coated on the front and back of the inorganic fiber cloth. The two layers are then stacked to form a layered structure of ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer-inorganic fiber cloth layer-ceramicized organosilicon layer. High-silica cloth is bonded to the ceramicized organosilicon layers on both sides. The cloth is shaped by a calender and vulcanized in a tunnel furnace in stages. The vulcanization zone temperatures are 80℃ for primary vulcanization foaming, 100℃ for secondary vulcanization foaming, 120℃ for tertiary vulcanization foaming, and 140℃ for quaternary vulcanization. The cloth is cooled and shaped by a shaping roller and then wound up to obtain a multi-layer fiber fireproof cloth based on ceramicized organosilicon.

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