A fireproof multilayer composite film, a thermal insulation felt and a preparation method thereof

Abstract

The present application relates to the technical field of fire-retardant thermal insulation materials, and discloses a fireproof multilayer composite film, a thermal insulation felt and a preparation method thereof.The fireproof multilayer composite film comprises a first polymer film layer, a first mesh cloth layer, an inorganic particle layer, a second mesh cloth layer and a second polymer film layer which are sequentially compounded; the first polymer film layer and the first mesh cloth layer and the second polymer film layer and the second mesh cloth layer are compounded together by an adhesive; the inorganic particle layer is compounded between the first mesh cloth layer and the second mesh cloth layer by an adhesive; wherein the inorganic particles in the inorganic particle layer are inorganic refractory materials, the particle size of the inorganic particles is 100-3000 mesh, and the aspect ratio is 1-10.The fireproof multilayer composite film has excellent anti-burn-through performance and excellent fireproof performance.

Description

Technical Field

[0001] This invention relates to the field of flame-retardant and heat-insulating materials technology, specifically to a fireproof multilayer composite film, a heat-insulating felt, and a method for preparing the same. Background Technology

[0002] According to statistics from the Cabin Safety Research and Technology Group (CRSTG), led by the FAA and with broad participation from the global civil aviation industry, 40% of passengers who survive an aircraft crash die in the subsequent fire. As the largest area in the aircraft cabin environment and the area with the most interaction with passengers, the fire resistance and flame retardancy of the cabin interior decoration significantly impact the safety of the occupants. Improving the fuselage's burn-through resistance, i.e., delaying the time it takes for flames to enter the cabin, provides sufficient time for emergency evacuation.

[0003] The sound and heat insulation materials used in existing commercial aircraft are usually installed on the rear side of the aircraft's interior panels. They are mainly formed by wrapping flame-retardant inorganic materials with high-performance fire-retardant composite films, thereby protecting passengers, cargo and equipment from the effects of environmental conditions and engine noise, while preventing the heat and sound insulation layers from burning through and stopping the spread of fire.

[0004] For example, Chinese patent CN102405172B and French patent FR3126106A3 both disclose a sandwich-structured composite laminate, consisting of a polymer moisture-proof layer with a UL94 flame rating of V-0, an inorganic sheet layer with a certain aspect ratio, and a thermoplastic film layer with a UL94 flame rating of V-0. The difference between these two patents lies in the different parameter ranges disclosed. The polymer films on both sides serve to prevent moisture and reduce surface flame combustion, while the middle fireproof layer is composed of inorganic sheet material with a certain particle aspect ratio. However, an excessively high aspect ratio can reduce the flowability of the inorganic material, thereby decreasing the coating uniformity and forming more pores during stacking, thus reducing the compactness of the fireproof layer. In addition, particle shape and particle size distribution also affect flowability and stacking characteristics. Insufficiently uniform and compact particle stacking may lead to a decrease in fireproof stability.

[0005] Chinese patent CN105593016B discloses a flame-retardant laminate, comprising a first thin film; a second silica cloth; a third thin film; and an adhesive compound, containing at least one inorganic filler. This flame-retardant laminate uses dense high-silica fiber cloth as the fireproof layer, exhibiting higher flexibility than inorganic particle stacking layers, but it has higher manufacturing costs, requires more precise weaving techniques, and has lower fire-retardant stability.

[0006] Therefore, there is an urgent need to provide a new type of fire-resistant multilayer composite membrane that can improve the uniformity of structural quality and the stability of product performance while reducing manufacturing costs, while meeting the requirements of burn-through resistance. Summary of the Invention

[0007] The purpose of this invention is to address the above-mentioned problems by providing a fireproof multilayer composite film, a heat insulation felt, and a method for preparing the same.

[0008] To achieve its objective, the present invention employs the following technical solution:

[0009] A first aspect of the present invention provides a fire-resistant multilayer composite membrane, comprising a first polymer film layer, a first mesh fabric layer, an inorganic particle layer, a second mesh fabric layer, and a second polymer film layer sequentially laminated together; the first polymer film layer and the first mesh fabric layer, as well as the second polymer film layer and the second mesh fabric layer, are laminated together by an adhesive; the inorganic particle layer is laminated between the first mesh fabric layer and the second mesh fabric layer by an adhesive.

[0010] The inorganic particles in the inorganic particle layer are inorganic refractory materials, and the particle size of the inorganic particles is 100-3000 mesh, with an aspect ratio of 1-10.

[0011] Preferably, the material used to manufacture the first polymer film layer or the second polymer film layer is selected from polyetheretherketone, polyetherketoneketone, polyetherketone, polyester, polyimide, polyvinyl fluoride, polyamide, polytetrafluoroethylene, polyarylsulfone, polyesteramide, polyesterimide, polyethersulfone, polyphenylene sulfide, and ethylene trifluorochloroethylene.

[0012] The fire-resistant multilayer composite membrane has a basis weight of 75-135 g / m³. 2 The thickness is 0.2 to 0.46 mm.

[0013] Preferably, the first or second mesh fabric layer is a flat mesh fabric formed by weaving multiple strands of fiber yarn, and the fiber yarn material is selected from organic fibers and inorganic fibers;

[0014] The organic fibers include: PAI fiber, PBI fiber, PI fiber, PEEK fiber, PPS fiber, PTFE fiber, PSU fiber, PPSU fiber, and PEI fiber;

[0015] The inorganic fibers include: glass fiber, high silica fiber, quartz fiber, basalt fiber, and alkaline earth silicate fiber;

[0016] The thickness of the first or second mesh layer is 50–120 μm, and the mass per unit area is 5–30 g / m². 2 The mesh size of the fabric is 6-18 mesh, and the tensile strength is 85-273 N / 50 mm.

[0017] During the composite process, the meshes of the first and second mesh layers are arranged alternately and do not completely overlap.

[0018] Preferably, the glass melting rate constant τ of the inorganic particles is ≥4;

[0019] The raw material sources for inorganic particles include: mica, vermiculite, talc, montmorillonite, feldspar, glass fiber, ceramic fiber, titanium dioxide, and fumed silica.

[0020] Preferably, the adhesive comprises 15-36% by mass in the fire-resistant multilayer composite film;

[0021] Adhesives include binders, wherein the binders are selected from one or more of the following: polyurethane, acrylic acid, vinyl acetate, aluminum silicate, and methyl silicone;

[0022] Preferred adhesives also include one or more of the following excipients: waterproofing agents, flame retardants, and defoamers;

[0023] The waterproofing agent is selected from one or more of the following: silicone-based waterproofing agents, fluorocarbon-based waterproofing agents, and acrylic-based waterproofing agents.

[0024] A second aspect of the present invention provides a method for preparing the above-mentioned fire-retardant multilayer composite film, comprising the following steps:

[0025] The first polymer film layer and the first mesh fabric layer are bonded together with an adhesive.

[0026] The second polymer film layer and the second mesh fabric layer are bonded together with an adhesive.

[0027] An inorganic particle mixture is coated onto a first mesh fabric layer and / or a second mesh fabric layer, and then dried and shaped to obtain an inorganic particle layer.

[0028] Fire-resistant multilayer composite film is prepared by bonding the various layers with adhesives and sandwiching the inorganic particle layer between the first and second mesh fabric layers.

[0029] The above-mentioned method for preparing fireproof multilayer composite film, wherein the inorganic particle mixture comprises: 35-65 wt% inorganic particles, 1-10 wt% binder, 0-15 wt% waterproofing agent, 0-10 wt% flame retardant, 0-1 wt% defoamer, and the balance being water.

[0030] A third aspect of the present invention provides a fireproof and heat-insulating felt comprising at least two fireproof multilayer composite films as described in any one of the above claims, wherein a core material layer is disposed between each pair of fireproof multilayer composite films, and the fireproof multilayer composite films and the core material layers are bonded together by an adhesive.

[0031] Preferably, the core material layer is selected from foam, organic or inorganic fibers;

[0032] The preferred materials for preparing the core layer are selected from polyimide foam, glass fiber, polyacrylonitrile fiber, carbon fiber, and pre-oxidized fiber;

[0033] The core material layer thickness is preferably 10–75 mm.

[0034] The fourth aspect of the present invention provides a method for preparing the above-mentioned fireproof and heat-insulating felt, comprising the following steps: placing two fireproof multilayer composite films opposite each other to cover the core material layer, and then bonding them together by adhesive and hot pressing to obtain the fireproof and heat-insulating felt.

[0035] The beneficial effects of this invention are:

[0036] The fire-resistant multilayer composite membrane of this invention includes an inorganic particle layer. During the preparation process, some inorganic particles fill or embed in the mesh of the mesh fabric, while other inorganic particles are attached to the surface of the constituent fibers of the mesh fabric. The inorganic particles fully encapsulate the constituent fibers of the mesh fabric, giving the composite membrane a good density and stability in its static structure. Even if the composite membrane is damaged or destroyed (such as when the mesh fabric fibers melt at high temperatures or due to mechanical damage), the inorganic particle layer can maintain the structural integrity (structural uniformity) of the composite membrane, avoiding adverse effects such as leakage points at fiber defects, and providing reliable fire protection.

[0037] The fire-resistant multilayer composite membrane of this invention uses a mesh fabric for its grid layer, which has lower material requirements. While meeting the requirements for burn-through resistance, it effectively reduces manufacturing costs and enhances market competitiveness. The resulting fire-resistant multilayer composite membrane, while meeting burn-through resistance requirements, improves structural uniformity, exhibits good overall strength and stability, and reduces manufacturing costs. Attached Figure Description

[0038] Figure 1 This is a schematic diagram of the structure of the fireproof multilayer composite film of the present invention;

[0039] Figure 2 This is a schematic diagram of the structure of the fireproof and heat-insulating felt of the present invention;

[0040] In the picture,

[0041] 1-Fireproof multilayer composite membrane, 111-First polymer membrane layer, 121-First mesh fabric layer, 13-Inorganic particle layer, 131-First inorganic particle layer, 132-Second inorganic particle layer, 122-Second mesh fabric layer, 112-Second polymer membrane layer;

[0042] 3-Fireproof and heat-insulating felt, 2-Core material layer. Detailed Implementation

[0043] The present invention will be further described below with reference to embodiments, but these embodiments are not intended to limit the scope of the invention.

[0044] Unless otherwise specified, the experimental methods described in the following examples are conventional methods.

[0045] Example 1: The fire-resistant multilayer composite film of the present invention

[0046] I. The fire-resistant multilayer composite film of the present invention

[0047] like Figure 1 The fire-resistant multilayer composite membrane 1 of the present invention, as shown, comprises a first polymer film layer 111, a first mesh fabric layer 121, an inorganic particle layer 13, a second mesh fabric layer 122, and a second polymer film layer 112, sequentially laminated together. Optionally, an adhesive layer is further provided on the outer side of the first polymer film layer 111 or the second polymer film layer 112. The first polymer film layer 111 and the first mesh fabric layer 121, as well as the second polymer film layer 112 and the second mesh fabric layer 122, are bonded together by adhesive. The inorganic particle layer 13 is laminated between the first mesh fabric layer 121 and the second mesh fabric layer 122 by adhesive.

[0048] In some embodiments, the inorganic particle layer 13 includes a first inorganic particle layer 131 and a second inorganic particle layer 132. A first polymer film layer 111, a first mesh fabric layer 121, and the first inorganic particle layer 131 are sequentially composited to form a first combined layer. A second polymer film layer 112, a second mesh fabric layer 122, and a second inorganic particle layer 132 are sequentially composited to form a second combined layer. The first inorganic particle layer 131 and the second inorganic particle layer 132 are bonded together with an adhesive, thereby bonding the first combined layer and the second combined layer together to form the fire-retardant multilayer composite film 1 of the present invention.

[0049] The fire-retardant multilayer composite membrane of this invention has a basis weight of 75-135 g / m³. 2 The thickness is 0.2 to 0.46 mm.

[0050] (1) Polymer film layer

[0051] The thickness of the first or second polymer film layer is 6 to 10 μm, preferably 6 μm. The manufacturing material of the first or second polymer film layer is selected from polyetheretherketone (PEEK), polyetherketoneketone (PEKK), polyetherketone (PEK), polyester, polyimide, polyvinyl fluoride, polyamide, polytetrafluoroethylene, polyarylsulfone, polyesteramide, polyesterimide, polyethersulfone, polyphenylene sulfide, ethylene trifluorochloroethylene, etc., and its surface combustion characteristics meet the ASTM E84 Class A standard issued by the American ASTM International Standardization Organization.

[0052] (2) Mesh Fabric Layer

[0053] The first mesh layer / second mesh layer is a flat mesh fabric formed by weaving multiple strands of fiber yarns. The fiber yarn material can be organic fiber or inorganic fiber.

[0054] Organic fibers include: PAI fiber, PBI fiber, PI fiber, PEEK fiber, PPS fiber, PTFE fiber, PSU fiber, PPSU fiber, and PEI fiber.

[0055] Inorganic fibers include: glass fiber, high silica fiber, quartz fiber, basalt fiber, and alkaline earth silicate fiber.

[0056] The specifications / performance parameters of the first or second mesh fabric layer are as follows:

[0057] The thickness is 50–120 μm, preferably 100 μm;

[0058] The mass per unit area is 5–30 g / m² 2 The preferred unit area mass is 15g / m². 2 ;

[0059] The mesh count of the mesh fabric is 6 to 18 meshes, and the mesh can be rectangular, circular, elliptical or polygonal, etc. The preferred mesh shape is rectangular, the preferred mesh size is (1 to 3 × 1 to 3) mm, and more preferably 3 × 3 mm;

[0060] The tensile strength is 85-273 N / 50 mm, with a preferred tensile strength of 150 N / 50 mm.

[0061] The mesh fabric layer can increase the coating uniformity of the inorganic particle layer and can also serve as a reinforcing material to provide mechanical support.

[0062] (3) Inorganic particle layer

[0063] The inorganic particle layer consists of high-temperature resistant inorganic particles. At a microscopic level, the inorganic particles fully encapsulate the constituent fibers of the mesh fabric to improve the structural density and fire resistance of the composite membrane.

[0064] The performance parameters of the inorganic particles are as follows:

[0065]

[0066] The particle size of inorganic particles should be between 100 and 3000 mesh. If the mesh number is too high, the particles will be too small and cannot overlap with the fiber surface of the mesh fabric layer; if the mesh number is too low, the particles will be too large and cannot fill the mesh of the mesh fabric.

[0067] The aspect ratio of inorganic particles should be between 1 and 10. As the aspect ratio gradually increases, the shape of the particles gradually becomes longer. If particles with an excessively large aspect ratio are used to prepare composite membranes, the inorganic particles cannot be effectively overlapped, resulting in pores in the inorganic particle layer. When the resulting fireproof membrane is exposed to flames, it is prone to leaks.

[0068] The glass melting rate constant τ of the inorganic particle layer is ≥4. The glass melting rate constant τ is a characteristic value representing the relative refractory nature of the inorganic particles in the composite film. The smaller the τ value, the lower the melting temperature. It can be calculated from the mass percentage of oxides in the inorganic particle layer, such as:

[0069]

[0070] (Contains boron);

[0071] (Contains lead);

[0072] Among them, SiO2, Al2O3, Na2O, K2O, B2O3, PbO, etc. represent the mass percentage (wt%) of oxides in the glass.

[0073] SiO2 provides glass with thermal stability, heat resistance, chemical stability, and mechanical strength, but higher SiO2 content requires higher melting temperatures and may lead to crystallization. Al2O3 can reduce the tendency of glass to crystallize and improve its chemical stability, thermal stability, and mechanical strength.

[0074] The raw materials for inorganic particles are inorganic refractory materials, which can be mineral materials, such as inorganic mineral materials whose main components are SiO2, Al2O3, etc., such as mica, vermiculite, talc, montmorillonite, feldspar, etc., or artificially synthesized high-temperature resistant inorganic materials, such as high-temperature resistant micro glass fibers, etc.

[0075] The main chemical components of common vermiculite raw materials are as follows: by mass percentage, 37-43% SiO2, 9-17% Al2O3, 5-24% Fe2O3, 11-23% MgO, 11.8% K2O, and 0.5-9% H2O.

[0076] The main chemical composition of glass fiber can be as follows: by mass percentage, 45.3% SiO2, 51.3% Al2O3, and 3.4% ZrO2.

[0077] The main chemical components of muscovite are as follows: by mass percentage, 45.2% SiO2, 38.5% Al2O3, 11.8% K2O, and 4.5% H2O.

[0078] (4) Adhesive

[0079] The adhesive used in the multilayer composite film of the present invention includes a binder, which is selected from one or more of the following: polyurethane, acrylic acid, vinyl acetate, aluminum silicate, and methyl organosilicon.

[0080] Adhesives may also contain one or more of the following additives: waterproofing agents, flame retardants, and defoamers. Among them, flame retardants and defoamers mainly play a role in enhancing fire resistance and flame retardancy.

[0081] The waterproofing agent is selected from one or more of the following: silicone-based waterproofing agents, fluorocarbon-based waterproofing agents, and acrylic-based waterproofing agents.

[0082] The adhesive accounts for 15-36% of the total mass of the multilayer composite film product of this invention.

[0083] II. The fireproof and heat-insulating felt of the present invention

[0084] The fire-resistant multilayer composite film of the present invention can also be used to prepare fire-resistant and heat-insulating felt:

[0085] like Figure 2 The fireproof and heat-insulating felt 3 of the present invention shown includes at least two fireproof multilayer composite films 1, with a core material layer 2 disposed between each pair of fireproof multilayer composite films 1, and the fireproof multilayer composite films 1 and the core material layer 2 are bonded together by an adhesive.

[0086] The core layer 2 is made of materials including foam, organic or inorganic fibers, such as polyimide foam, glass fiber, polyacrylonitrile fiber, carbon fiber, pre-oxidized fiber, etc. The thickness of the core layer 2 is 10-75 mm.

[0087] The number of fire-resistant multilayer composite membranes 1 can be multiple (e.g., three or five), with core material layers 2 set between each pair, forming a sandwich structure in which the fire-resistant multilayer composite membrane 1 is sandwiched with the core material layer 2.

[0088] The method for preparing the fireproof and heat-insulating felt of the present invention is as follows: an adhesive is coated on the first polymer film layer 111 and / or the second polymer film layer 112 of the fireproof multilayer composite film 1, the fireproof multilayer composite films 1 are placed opposite each other, and the core material layer 2 is wrapped around them. The fireproof and heat-insulating felt 3 is obtained by adhesive bonding and hot pressing. The heat-insulating felt suitable for aircraft fuselage is obtained. The two fireproof multilayer composite film 1 products are not easy to peel off and delaminate after hot pressing and have good heat-sealing properties.

[0089] Example 2: Preparation method of the fire-retardant multilayer composite film of the present invention

[0090] I. Preparation of the fire-retardant multilayer composite film of Example 1

[0091] The first method for preparing a fire-resistant multilayer composite film includes the following steps:

[0092] The first polymer film layer and the first mesh fabric layer are bonded together with an adhesive.

[0093] The second polymer film layer and the second mesh fabric layer are bonded together with an adhesive.

[0094] An inorganic particle mixture is coated onto a first mesh fabric layer and / or a second mesh fabric layer, and then dried and shaped to obtain an inorganic particle layer.

[0095] Fire-resistant multilayer composite film is prepared by bonding the various layers with adhesives and sandwiching the inorganic particle layer between the first and second mesh fabric layers.

[0096] Preferably, the fire-retardant multilayer composite film of the present invention can also be prepared by the second preparation method, the steps of which are as follows:

[0097] Step 1: Bond the first polymer film layer and the first mesh fabric layer together with an adhesive; bond the second polymer film layer and the second mesh fabric layer together using the same method.

[0098] Step 2: Coat the first mesh fabric layer with an inorganic particle mixture, and dry and set it at high temperature to obtain the first inorganic particle layer. The first polymer film layer, the first mesh fabric layer, and the first inorganic particle layer constitute the first composite layer. Coat the second mesh fabric layer with an inorganic particle mixture, and dry and set it at high temperature to obtain the second inorganic particle layer. The second polymer film layer, the second mesh fabric layer, and the second inorganic particle layer constitute the second composite layer.

[0099] The inorganic particle mixture contains 35-65 wt% inorganic particles, 1-10 wt% binder, 0-15 wt% waterproofing agent, 0-10 wt% flame retardant, 0-1 wt% defoamer, and the balance is water.

[0100] Step 3: Apply adhesive to the inorganic particle layer of the first composite layer and the second composite layer, and hot-press the first composite layer and the second composite layer together to obtain a fireproof multilayer composite film.

[0101] Preferably, in the multilayer composite membrane, the first and second mesh fabric layers are arranged in an alternating pattern. This alternating arrangement means that the fiber lines of the mesh fabric layers in the same direction do not completely overlap. If the fiber lines completely overlap, one fiber line covers another, preventing the inorganic particles from fully encapsulating the fibers. Once the fibers melt due to heat, defects are more likely to occur at the overlapping points, increasing the risk of leaks and reducing the product's burn-through resistance.

[0102] In fire-resistant multilayer composite films, some inorganic particles are uniformly filled or embedded within the mesh of the mesh fabric, while others are attached to the surface of the constituent fibers of the mesh fabric. The mesh size should not be too large or too small. When the mesh size is too large, inorganic particles are more likely to aggregate at the mesh edges, intersections, or larger spaces within the mesh, forming particle clusters or agglomerates. Uneven distribution of inorganic particles leads to thinner areas where leakage points are easily formed at high temperatures, resulting in insufficient flame burn-through radiation temperature. When the mesh size is too small, it increases unnecessary weight and the processing difficulty of the staggered arrangement, which will also directly affect the coating effect of inorganic particles, making it difficult for inorganic particles to fully encapsulate the fibers. Since the temperature resistance of some mesh fibers is not as good as that of inorganic particles (except for high-silica fibers), the mesh melts at high temperatures, creating more pores, which reduces the flame burn-through resistance.

[0103] During the preparation of fire-resistant multilayer composite membranes, inorganic particles fully encapsulate the constituent fibers of the mesh fabric, giving the composite membrane a static structure with good density and stability. Even when the composite membrane is damaged or destroyed (such as when the mesh fabric fibers melt at high temperatures or due to mechanical damage), the inorganic particle layer can maintain the structural integrity (structural uniformity) of the composite membrane, avoiding adverse effects such as leakage points at fiber defects, and providing reliable fire protection.

[0104] The fire-resistant multilayer composite membrane of this invention uses a mesh fabric for its mesh layer, which has lower material requirements. While meeting the requirements for burn-through resistance, it effectively reduces production costs and enhances market competitiveness. The first polymer film layer, first mesh fabric layer, second mesh fabric layer, second polymer film layer, inorganic particulate material, and adhesive raw materials used in the composite membrane of this invention are all commercially available.

[0105] The composite membrane products in Table 1-2 are prepared according to the second preparation method described above.

[0106] Table 1

[0107]

[0108]

[0109] Table 2

[0110]

[0111]

[0112] *Note: The inorganic particle layer weight in Table 2 refers to the weight of the entire inorganic particle layer, consisting of the first inorganic particle layer and the second inorganic particle layer, per unit area of ​​the fireproof multilayer composite film product.

[0113] The inorganic particles used in Examples 1-9, Examples 11-15, and Comparative Examples 1-2 have the following composition by mass percentage: 41.73% SiO2, 12.54% Al2O3, 10.75% K2O, 0.21% Na2O, 0.45% CaO, 0.12% TFe2O3, 27.7% MgO, and 0.45% P2O5, derived from fluorophlogopite.

[0114] The inorganic particles of Example 10 have the following composition by mass percentage: 42.44% SiO2, 6.40% K2O, 4.21% Na2O, 45.95% BaO / C, and 1.00% BaO / N, and are derived from silicate glass.

[0115] The inorganic particles of Comparative Example 3 are composed of, by mass percentage: 41.19% SiO2, 13.81% Al2O3, 14.31% K2O, 11.80% Na2O, 0.32% CaO, 9.89% Fe2O3, and 9.13% H2O, and are derived from feldspar.

[0116] The inorganic particles of Comparative Example 4 consist of the following components by mass percentage: 38.62% SiO2, 14.78% Al2O3, 9.41% Fe2O3, 22.16% MgO, 6.29% K2O, 2.02% Na2O, 1.45% CaO, and 5.27% H2O, and are derived from vermiculite.

[0117] In the products of the embodiments and comparative examples, the polymer types of the first polymer film layer and the second polymer film layer of each product are the same, that is, the raw materials of the polymer film layers of the products are the same, and the mesh fabrics used in the first mesh fabric layer and the second mesh fabric layer are also the same. However, it should be understood that the above embodiments and comparative examples are not intended to limit the present invention. In some embodiments, the first polymer film and the second polymer film have different polymer types; similarly, the mesh fabrics of the first mesh fabric layer and the second mesh fabric layer may also have different specifications.

[0118] II. Fireproof membrane performance testing

[0119] The test methods or reference standards for the performance indicators of fire-resistant multilayer composite films are as follows:

[0120] Burn-through resistance test: The test shall be conducted in accordance with Part VII of Appendix F of the Airworthiness Standards for Transport Category Aircraft (CCAR25) formulated by the Civil Aviation Administration of China (CAAC). The requirements are: neither of the two specimens shall be burned through by fire or flame within 4 minutes; or, the heat flux of either specimen at a point 30.5 cm (12 inches) from the test fixture surface on the side insulated from the cold side shall not exceed 2.27 W / cm². 2 (2.0 British thermal units / foot) 2 Second).

[0121] Test method for heat sealability (peel strength): ISO 11339.

[0122] Test method for tear resistance: ISO 13937-2.

[0123] Water resistance test method: In one test, a sample of fire-resistant multilayer composite membrane was weighed and then completely immersed in water at 23°C for 72 hours. After this period, the sample was weighed again, and the water absorption rate was calculated.

[0124] Test method for burst strength: Federal Standard Test Method FED-STD-191METHOD 5122.

[0125] The test results are shown in Table 3:

[0126] Table 3

[0127]

[0128]

[0129] As shown in Table 1-3, Comparative Example 1, due to its excessively large mesh size (5mm*5mm), exhibited uneven distribution of inorganic particles. Areas with thinner inorganic particles were prone to leaks at high temperatures, resulting in the fire-retardant multilayer composite film product failing to meet burn-through resistance standards. Specifically, the mesh edges are prominent points in the mesh structure, making it easier for particles to deposit and aggregate during solution flow or drying. Furthermore, the large mesh size provides more space for particle movement during coating, potentially leading to the formation of large agglomerates within the mesh, especially in the center or near the edges, all of which reduce the product's burn-through resistance.

[0130] Comparative Example 2 has an excessively small mesh size, resulting in a high basis weight for the fire-resistant multilayer composite film product, which does not meet the requirements for lightweight and is unsuitable for applications such as aircraft and trains where lightweight fire-resistant films are required. Comparative Example 3, on the other hand, suffers from a glass melting rate constant τ < 4 in its inorganic particle layer, causing the fire-resistant multilayer composite film product to fail to meet the burn-through resistance standard.

[0131] Comparative Example 4 is a sample prepared according to Example 2 of Chinese Patent CN102405172B. The structure of the fireproof film in Comparative Example 4 is different from that of the fireproof film of the present invention. Even though the inorganic particles in Comparative Example 4 have better temperature resistance (τ=6.426), their burn-through resistance is still lower than that of Example 2, with a maximum heat flux of 2.21 W / cm². 2 Near failure (2.27W / cm) 2 Furthermore, the strength of Comparative Example 4 was also much lower than that of Example 2.

[0132] The fireproof membrane products of Examples 1-15 have excellent burn-through resistance, as well as excellent tear resistance, burst strength and lightweight properties.

Claims

1. A fire-resistant multilayer composite membrane, characterized in that, The assembly comprises a first polymer film layer, a first mesh fabric layer, an inorganic particle layer, a second mesh fabric layer, and a second polymer film layer, which are sequentially laminated together. The first polymer film layer and the first mesh fabric layer, as well as the second polymer film layer and the second mesh fabric layer, are bonded together by an adhesive. The inorganic particle layer is bonded between the first mesh fabric layer and the second mesh fabric layer by an adhesive. Among them, the inorganic particles in the inorganic particle layer are inorganic refractory materials, the particle size of the inorganic particles is 100~3000 mesh, the aspect ratio is 1~10, and the glass melting rate constant τ of the inorganic particles is ≥4. The thickness of the first or second mesh layer is 50–120 μm, and the mass per unit area is 5–30 g / m². 2 The mesh size is 1~3×1~3 mm, and the tensile strength is 85~273 N / 50mm; when composited, the meshes of the first mesh layer and the second mesh layer are arranged alternately and do not completely overlap. The fire-resistant multilayer composite membrane has a basis weight of 75~135g / m³. 2 The thickness is 0.2~0.46mm.

2. The fire-resistant multilayer composite membrane according to claim 1, characterized in that, The material used to manufacture the first polymer film layer or the second polymer film layer is selected from polyetheretherketone, polyetherketoneketone, polyetherketone, polyester, polyimide, polyvinyl fluoride, polyamide, polytetrafluoroethylene, polyarylsulfone, polyesteramide, polyesterimide, polyethersulfone, polyphenylene sulfide, and ethylene trifluorochloroethylene.

3. The fire-retardant multilayer composite membrane according to claim 1, characterized in that, The first or second mesh fabric layer is a flat mesh fabric formed by weaving multiple strands of fiber yarns, and the fiber yarn material is selected from organic fibers and inorganic fibers. The organic fibers include: PAI fiber, PBI fiber, PI fiber, PEEK fiber, PPS fiber, PTFE fiber, PSU fiber, PPSU fiber, and PEI fiber; The inorganic fibers include: glass fiber, high silica fiber, quartz fiber, basalt fiber, and alkaline earth silicate fiber.

4. The fire-retardant multilayer composite membrane according to claim 1, characterized in that, The raw material sources for the inorganic particles include: mica, vermiculite, talc, montmorillonite, glass fiber, ceramic fiber, titanium dioxide, and fumed silica.

5. The fire-retardant multilayer composite membrane according to claim 1, characterized in that, The adhesive in the fire-resistant multilayer composite film has a mass percentage of 15-36%. Adhesives include binders selected from one or more of the following: polyurethane, acrylic acid, vinyl acetate, aluminum silicate, and methyl silicone.

6. The fire-retardant multilayer composite membrane according to claim 5, characterized in that: The adhesive also includes one or more excipients selected from waterproofing agents, flame retardants, and defoamers; The waterproofing agent is selected from one or more of the following: silicone-based waterproofing agents, fluorocarbon-based waterproofing agents, and acrylic-based waterproofing agents.

7. The method for preparing the fire-retardant multilayer composite film according to any one of claims 1 to 6, characterized in that, Includes the following steps: The first polymer film layer and the first mesh fabric layer are bonded together with an adhesive. The second polymer film layer and the second mesh fabric layer are bonded together with an adhesive. An inorganic particle mixture is coated onto a first mesh fabric layer and / or a second mesh fabric layer, and then dried and shaped to obtain an inorganic particle layer. Fire-resistant multilayer composite film is prepared by bonding the various layers with adhesives and sandwiching the inorganic particle layer between the first and second mesh fabric layers.

8. The method for preparing the fire-retardant multilayer composite film according to claim 7, characterized in that, The inorganic particle mixture comprises: 35-65 wt% inorganic particles, 1-10 wt% binder, 0-15 wt% waterproofing agent, 0-10 wt% flame retardant, 0-1 wt% defoamer, and the balance being water.

9. A fireproof and heat-insulating felt, characterized in that: It includes at least two fire-resistant multilayer composite films as described in any one of claims 1 to 6, wherein a core material layer is disposed between each pair of fire-resistant multilayer composite films, and the fire-resistant multilayer composite films and the core material layers are bonded together by an adhesive.

10. The fireproof and heat-insulating felt according to claim 9, characterized in that: The core material is selected from foam, organic or inorganic fibers.

11. The fireproof and heat-insulating felt according to claim 10, characterized in that: The core material is prepared from polyimide foam, glass fiber, polyacrylonitrile fiber, carbon fiber, and pre-oxidized fiber. The core material layer thickness is 10~75 mm.

12. The method for preparing the fireproof and heat-insulating felt according to any one of claims 9 to 11, characterized in that, The process includes the following steps: placing two fire-resistant multilayer composite films opposite each other to cover the core material layer, and then bonding them together with adhesive and hot pressing to obtain the fire-resistant and heat-insulating felt.

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