Heat-sealable flame-retardant fluorine-containing composite film as well as preparation method and application thereof

Abstract

The invention provides a heat-sealable and flame-retardant composite film. The heat-sealable and flame-retardant composite film comprises an aluminized film, a flame-retardant net film and a reinforced grid which are sequentially compounded, the flame-retardant net film comprises the following components in parts by weight: 40-60 parts of polyamide resin, 10-20 parts of EBA resin, 5-10 parts of a first flame retardant, 5-10 parts of a second flame retardant, 5-10 parts of a third flame retardant, 5-10 parts of a tackifier and 1-2 parts of an antioxidant. The first flame retardant comprises brominated polystyrene and / or brominated epoxy resin; the second flame retardant comprises sodium antimonate and / or sodium antimonate; the third flame retardant comprises zinc borate and / or zinc phosphate. The fluorine-containing composite film prepared by the invention has the characteristics of heat sealability, flame retardance and high barrier property, and also has the characteristics of easiness in continuous processing, uniform dispersion of the flame retardant, no use of a solvent, good performance consistency and the like. The heat-sealable and flame-retardant fluorine-containing composite film prepared by the invention has a wide application prospect in a heat-insulating and sound-insulating system of an airplane.

Description

Technical Field

[0001] This invention belongs to the field of composite material technology, and particularly relates to a heat-sealable, flame-retardant composite film, its preparation method and application. Background Technology

[0002] Aircraft fuselages commonly use heat- and sound-insulating materials. These materials function to create a barrier against flame transmission and to reduce external noise, thereby minimizing noise entering the cabin from the outside and maintaining a suitable temperature inside the cabin.

[0003] Foreign countries began focusing on the design, manufacturing, installation, and material development of thermal / sound insulation systems as early as the 1950s. They have achieved advanced levels in noise level prediction and simulation, sound insulation models, and testing, enabling them to develop complete thermal / sound insulation system solutions for different aircraft models. Fluorinated composite films used in thermal / sound insulation systems generally consist of multi-layered composite structures, possessing heat-sealable, flame-retardant, and high-barrier properties. The core technology lies in the preparation and lamination of heat-sealable, flame-retardant adhesives. Currently, the domestic production of composite films for thermal / sound insulation systems mainly adopts the solution lamination method. However, in continuous production, the solution lamination process suffers from problems such as easy sedimentation of flame retardants, difficulty in dispersion, difficulty in solvent removal, and high production costs. Therefore, there is an urgent need to develop a green and efficient method for preparing fluorinated composite films. Summary of the Invention

[0004] The purpose of this invention is to provide a heat-sealable, flame-retardant composite film, its preparation method and application. The composite film of this invention has the characteristics of easy continuous processing, uniform dispersion of flame retardant and good performance consistency.

[0005] This invention provides a heat-sealable, flame-retardant composite film, comprising an aluminized film, a flame-retardant mesh, and a reinforcing mesh sequentially laminated together;

[0006] The flame-retardant mesh comprises the following components in parts by weight:

[0007] 40-60 parts of polyamide resin, 10-20 parts of EBA resin, 5-10 parts of first flame retardant, 5-10 parts of second flame retardant, 5-10 parts of third flame retardant, 5-10 parts of tackifier, and 1-2 parts of antioxidant.

[0008] The first flame retardant comprises brominated polystyrene and / or brominated epoxy resin; the second flame retardant comprises sodium metaantimonate and / or sodium antimonate; and the third flame retardant comprises zinc borate and / or zinc phosphate.

[0009] Preferably, the polyamide resin has a melt viscosity of 2000~4500 mPa·s and a melt index of 50~100 g / 10 min.

[0010] Preferably, the butyl acrylate content in the EBA resin is 20-30 wt%, and the melt index is 50-100 g / 10 min.

[0011] Preferably, the tackifier comprises one or more of rosin resin, terpene resin, and petroleum resin;

[0012] The antioxidants include one or more of β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, dilauryl thiodipropionate, and tris(2,4-di-tert-butyl)phosphite.

[0013] Preferably, the aluminized film includes an aluminized PVF film, an aluminized ETFE film, or an aluminized PVDF film;

[0014] The reinforcing mesh is made of one or more of nylon 66, polyimide, and liquid crystal polymer.

[0015] This invention provides a method for preparing the heat-sealable, flame-retardant composite film as described above, comprising the following steps:

[0016] A) Polyamide resin, EBA resin, first flame retardant, second flame retardant, third flame retardant, tackifier and antioxidant are melt-mixed, extruded and granulated to obtain flame retardant masterbatch;

[0017] B) The flame-retardant masterbatch is melt-blown into a mesh to obtain a flame-retardant mesh film;

[0018] C) The aluminum-coated film, flame-retardant mesh, and reinforcing mesh are combined to obtain a heat-sealable, flame-retardant composite film.

[0019] Preferably, in step A), an extruder is used for granulation, the temperature of the melt mixing is 220~250℃, and the screw speed is 40~70rpm.

[0020] Preferably, in step B), the melt-blown web forming temperature is 230~260℃, the spinneret diameter is 0.1~0.15mm, the receiving distance is 10~15cm, and the basis weight of the flame-retardant web is 8~14g / cm³. 2 .

[0021] Preferably, in step C), lamination is used, and the lamination pressure is 0.25~0.4MPa and the temperature is 140~170℃.

[0022] This invention provides the application of the heat-sealable, flame-retardant composite film as described above in aircraft thermal and sound insulation systems.

[0023] This invention provides a heat-sealable, flame-retardant composite film, comprising an aluminized film, a flame-retardant mesh, and a reinforcing mesh sequentially laminated together. The flame-retardant mesh comprises the following components in parts by weight: 40-60 parts polyamide resin, 10-20 parts EBA resin, 5-10 parts first flame retardant, 5-10 parts second flame retardant, 5-10 parts third flame retardant, 5-10 parts tackifier, and 1-2 parts antioxidant. The first flame retardant comprises brominated polystyrene and / or brominated epoxy resin; the second flame retardant comprises sodium metaantimonate and / or sodium antimonate; and the third flame retardant comprises zinc borate and / or zinc phosphate. This invention improves the peel strength between the polyamide hot melt adhesive and the aluminized film by adding EBA resin and tackifier to the polyamide matrix, enhances the wettability of the polyamide to the reinforcing mesh, thereby increasing the heat-sealing strength of the fluorinated composite film, and simultaneously improves the flame-retardant performance of the mesh by adding synergistic flame retardants. This invention prepares a fluorinated composite membrane through processes including flame-retardant masterbatch preparation, flame-retardant web processing, and multilayer lamination. The fluorinated composite membrane possesses heat-sealable, flame-retardant, and high barrier properties, while also exhibiting advantages such as easy continuous processing, uniform dispersion of the flame retardant, solvent-free operation, and good performance consistency. The heat-sealable, flame-retardant fluorinated composite membrane prepared by this invention has broad application prospects in aircraft thermal and sound insulation systems. Detailed Implementation

[0024] This invention provides a heat-sealable, flame-retardant composite film, comprising an aluminized film, a flame-retardant mesh, and a reinforcing mesh sequentially laminated together;

[0025] The flame-retardant mesh comprises the following components in parts by weight:

[0026] 40-60 parts of polyamide resin, 10-20 parts of EBA resin, 5-10 parts of first flame retardant, 5-10 parts of second flame retardant, 5-10 parts of third flame retardant, 5-10 parts of tackifier, and 1-2 parts of antioxidant.

[0027] The first flame retardant comprises brominated polystyrene and / or brominated epoxy resin; the second flame retardant comprises sodium metaantimonate and / or sodium antimonate; and the third flame retardant comprises zinc borate and / or zinc phosphate.

[0028] In this invention, the melt viscosity of the polyamide resin is preferably 2000~4500 mPa·s, more preferably 2500~4000 mPa·s, and the melt index is preferably 50~100 g / 10min, more preferably 60~80 g / 10min; the weight parts of the polyamide resin are preferably 40~60 parts, more preferably 45~55 parts, such as 40 parts, 41 parts, 42 parts, 43 parts, 44 parts, 45 parts, 46 parts, 47 parts, 48 ​​parts, 49 parts, 50 parts, 51 parts, 52 parts, 53 parts, 54 parts, 55 parts, 56 parts, 57 parts, 58 parts, 59 parts, 60 parts, preferably within the range of any of the above values ​​as the upper or lower limit.

[0029] In this invention, the butyl acrylate content in the EBA resin (ethylene butyl acrylate resin) is preferably 20-30 wt%, more preferably 22-28 wt%, such as 20 wt%, 21 wt%, 22 wt%, 23 wt%, 24 wt%, 25 wt%, 26 wt%, 27 wt%, 28 wt%, 29 wt%, 30 wt%, preferably within the range of any of the above values ​​as the upper or lower limit. The melt index of the EBA resin is preferably 50-100 g / 10 min, more preferably 60-80 g / 10 min. The weight parts of the EBA resin are preferably 10-20 parts, such as 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, preferably within the range of any of the above values ​​as the upper or lower limit.

[0030] In this invention, the first flame retardant preferably includes brominated polystyrene and / or brominated epoxy resin; the weight parts of the first flame retardant are preferably 5 to 10 parts, such as 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, preferably within the range of any of the above values ​​as the upper or lower limit.

[0031] In this invention, the second flame retardant includes sodium metaantimonate and / or sodium antimonate; the weight of the second flame retardant is preferably 5 to 10 parts, such as 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, preferably within the range of any of the above values ​​as the upper or lower limit.

[0032] In this invention, the third flame retardant includes zinc borate and / or zinc phosphate; the weight of the third flame retardant is preferably 5 to 10 parts, such as 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, preferably within the range of any of the above values ​​as the upper or lower limit.

[0033] Specifically, in some embodiments of the present invention, the mass ratio of the first flame retardant, the second flame retardant and the third flame retardant is preferably 1:1:1.

[0034] In this invention, the tackifier preferably includes one or more of rosin resin, terpene resin and petroleum resin; the weight fraction of the tackifier is preferably 5 to 10 parts, such as 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, preferably within the range of any of the above values ​​as the upper or lower limit.

[0035] In this invention, the antioxidant includes one or more of β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, dilauryl thiodipropionate, and tris(2,4-di-tert-butyl)phosphite; the antioxidant is preferably present in 1 to 2 parts by weight.

[0036] In this invention, the basis weight of the flame-retardant mesh is preferably 8~14 g / cm³. 2 More preferably 9~12 g / cm³ 2 .

[0037] In this invention, the aluminized film preferably comprises an aluminized layer and a substrate layer, wherein the substrate layer is preferably a PVF film, an ETFE film, or a PVDF film; the thickness of the substrate layer is preferably 12~18μm, more preferably 15~16μm; the thickness of the aluminized layer is preferably 100~200nm, more preferably 120~180nm, such as 100 nm, 120 nm, 150 nm, 180 nm, 200 nm, preferably within the range of any of the above values ​​as the upper or lower limit; the aluminized layer of the aluminized film is in contact with the flame-retardant mesh film.

[0038] In this invention, the reinforcing mesh is preferably made of one or more of nylon 66, polyimide, and liquid crystal polymer; the mesh size is preferably 2-4 mm; and the basis weight of the reinforcing mesh is preferably 5-10 g / m³. 2 .

[0039] This invention also provides a method for preparing the heat-sealable, flame-retardant composite film described above, comprising the following steps:

[0040] A) Polyamide resin, EBA resin, first flame retardant, second flame retardant, third flame retardant, tackifier and antioxidant are melt-mixed, extruded and granulated to obtain flame retardant masterbatch;

[0041] B) The flame-retardant masterbatch is melt-blown into a mesh to obtain a flame-retardant mesh film;

[0042] C) The aluminum-coated film, flame-retardant mesh, and reinforcing mesh are combined to obtain a heat-sealable, flame-retardant composite film.

[0043] In this invention, the types and amounts of the polyamide resin, EBA resin, first flame retardant, second flame retardant, third flame retardant, tackifier, and antioxidant are the same as those described above, and will not be repeated here.

[0044] The present invention preferably involves adding the above materials into an extruder according to the specified ratio, melting and mixing them, and then underwater pelletizing them to obtain flame retardant masterbatch.

[0045] In this invention, the temperature of the melt mixing is preferably 220~250℃, more preferably 230~240℃, such as 220℃, 225℃, 230℃, 235℃, 240℃, 245℃, 250℃, preferably a range of values ​​with any of the above values ​​as the upper or lower limit; during the melt mixing process, the screw speed of the extruder is preferably 40~70 rpm, more preferably 50~60 rpm.

[0046] After obtaining the flame retardant masterbatch, the present invention adds the flame retardant masterbatch into an extruder and heats and melts it again. The melt passes through a metering pump and reaches the spinneret. Compressed air is applied to the melt polymer to draw it into filaments. The fibers are cooled and solidified into a web to obtain a flame retardant web film.

[0047] In this invention, the heating and melting temperature is preferably 230~260℃, more preferably 240~250℃, such as 230℃, 235℃, 240℃, 245℃, 250℃, 255℃, 260℃, preferably a range of values ​​with any of the above as the upper or lower limit; the spinneret orifice size is preferably 0.1~0.15mm, the number of spinneret orifices is preferably 1000~2000, and the receiving distance for meltblown web is preferably 10~15cm.

[0048] After obtaining the flame-retardant mesh film, the present invention sequentially unwinds the aluminum-coated film, the flame-retardant mesh film, and the reinforcing mesh, and performs lamination to obtain a heat-sealable, flame-retardant fluorine-containing composite film.

[0049] In this invention, during the lamination process, the temperature of the pressure roller is preferably 140~170℃, more preferably 150~160℃, such as 140℃, 145℃, 150℃, 155℃, 160℃, 165℃, 170℃, preferably within the range of any of the above values ​​as the upper or lower limit; the lamination pressure is preferably 0.25~0.4MPa, more preferably 0.3~0.35MPa.

[0050] The present invention also provides an application of the heat-sealable, flame-retardant composite film described above in an aircraft thermal and sound insulation system.

[0051] This invention provides a heat-sealable, flame-retardant composite film, comprising an aluminized film, a flame-retardant mesh, and a reinforcing mesh sequentially laminated together. The flame-retardant mesh comprises the following components in parts by weight: 40-60 parts polyamide resin, 10-20 parts EBA resin, 5-10 parts first flame retardant, 5-10 parts second flame retardant, 5-10 parts third flame retardant, 5-10 parts tackifier, and 1-2 parts antioxidant. The first flame retardant comprises brominated polystyrene and / or brominated epoxy resin; the second flame retardant comprises sodium metaantimonate and / or sodium antimonate; and the third flame retardant comprises zinc borate and / or zinc phosphate. This invention improves the peel strength between the polyamide hot melt adhesive and the aluminized film by adding EBA resin and tackifier to the polyamide matrix, enhances the wettability of the polyamide to the reinforcing mesh, thereby increasing the heat-sealing strength of the fluorinated composite film, and simultaneously improves the flame-retardant performance of the mesh by adding synergistic flame retardants. This invention prepares a fluorinated composite membrane through processes including flame-retardant masterbatch preparation, flame-retardant web processing, and multilayer lamination. The fluorinated composite membrane possesses heat-sealable, flame-retardant, and high barrier properties, while also exhibiting advantages such as easy continuous processing, uniform dispersion of the flame retardant, solvent-free operation, and good performance consistency. The heat-sealable, flame-retardant fluorinated composite membrane prepared by this invention has broad application prospects in aircraft thermal and sound insulation systems.

[0052] To further illustrate the present invention, the following detailed description of a heat-sealable, flame-retardant composite film, its preparation method, and its application, in conjunction with embodiments, is provided by the present invention, but should not be construed as limiting the scope of protection of the present invention.

[0053] Example 1

[0054] (1) Preparation of flame retardant masterbatch:

[0055] 60 parts of polyamide resin with a melt viscosity of 4500 mPa∙s and a softening point of 115℃, 20 parts of EBA resin with a butyl acrylate content of 30 wt% and a melt index of 100 g / 10 min, 10 parts of brominated polystyrene, 10 parts of sodium metaantimonate, 10 parts of zinc borate, 10 parts of rosin resin, and 2 parts of octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate.

[0056] The materials are mixed according to the above ratio and added to the extruder. The temperature is controlled at 250℃ and the screw speed is controlled at 70rpm / min. After the materials are melted and mixed evenly, they are pelletized underwater to obtain flame retardant masterbatch.

[0057] (2) Flame-retardant mesh processing

[0058] Flame-retardant masterbatch is added to an extruder and reheated to melt at 260°C. The melt is then pumped through a metering pump to a spinneret with 0.15mm orifice size and 2000 orifices. Compressed air is applied to the molten polymer, drawing it into filaments. The fibers cool and solidify into a web. The preferred receiving distance for the melt-blown web is 15cm, and the basis weight of the flame-retardant web is 14g / m². 2 .

[0059] (3) Multilayer composite

[0060] A 18μm aluminum-coated 200nm PVF film, a flame-retardant mesh, a mesh size of 4mm, and a mesh weight of 5g / m² are used. 2 Nylon 66 reinforced mesh is unwound sequentially, and the pressure roller is heated to 140°C with the pressure controlled at 0.4MPa for lamination to obtain a heat-sealable, flame-retardant fluorinated composite film 1.

[0061] Example 2

[0062] (1) Preparation of flame retardant masterbatch:

[0063] 50 parts of polyamide resin with a melt viscosity of 3500 mPa∙s and a softening point of 110℃, 15 parts of EBA resin with a butyl acrylate content of 25 wt% and a melt index of 75 g / 10 min, 7.5 parts of brominated polystyrene, 7.5 parts of sodium metaantimonate, 7.5 parts of zinc borate, 7.5 parts of rosin resin, and 1.5 parts of octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate.

[0064] The materials are mixed according to the above ratio and added to the extruder. The temperature is controlled at 250℃ and the screw speed is controlled at 70rpm / min. After the materials are melted and mixed evenly, they are granulated underwater to obtain flame retardant masterbatch.

[0065] (2) Flame-retardant mesh processing

[0066] Flame-retardant masterbatch is added to an extruder and reheated to melt at 260°C. The melt is then pumped through a metering pump to a spinneret. The spinneret orifice size is preferably 0.15 mm, and the number of orifices is preferably 2000. Compressed air is applied to the molten polymer to draw it into filaments. The fibers cool and solidify into a web. The preferred receiving distance for the melt-blown web is 15 cm, and the basis weight of the flame-retardant web is 14 g / m². 2 .

[0067] (3) Multilayer composite

[0068] A 18μm aluminum-coated 200nm PVF film, a flame-retardant mesh, a mesh size of 4mm, and a mesh weight of 5g / m² are used. 2Nylon 66 reinforced mesh is unwound sequentially, and the pressure roller is heated to 140°C with the pressure controlled at 0.4MPa for lamination to obtain a heat-sealable, flame-retardant fluorinated composite film 2.

[0069] Example 3

[0070] 40 parts of polyamide resin with a melt viscosity of 2000 mPa∙s and a softening point of 100℃, 10 parts of EBA resin with a butyl acrylate content of 20 wt% and a melt index of 50 g / 10 min, 5 parts of brominated polystyrene, 5 parts of sodium metaantimonate, 5 parts of zinc borate, 5 parts of rosin resin, and 1 part of octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate.

[0071] The materials are mixed according to the above ratio and added to the extruder. The temperature is controlled at 250℃ and the screw speed is controlled at 70rpm / min. After the materials are melted and mixed evenly, they are granulated underwater to obtain flame retardant masterbatch.

[0072] (2) Flame-retardant mesh processing

[0073] Flame-retardant masterbatch is added to an extruder and reheated to melt at 260°C. The melt is then pumped through a metering pump to a spinneret. The spinneret orifice size is preferably 0.15 mm, and the number of orifices is preferably 2000. Compressed air is applied to the molten polymer to draw it into filaments. The fibers cool and solidify into a web. The preferred receiving distance for the melt-blown web is 15 cm, and the basis weight of the flame-retardant web is 14 g / m². 2 .

[0074] (3) Multilayer composite

[0075] A 18μm aluminum-coated 200nm PVF film, a flame-retardant mesh, a mesh size of 4mm, and a mesh weight of 5g / m² are used. 2 Nylon 66 reinforced mesh is unwound sequentially, and the pressure roller is heated to 140°C with the pressure controlled at 0.4MPa for lamination to obtain a heat-sealable, flame-retardant fluorinated composite film 3.

[0076] Example 4

[0077] (1) Preparation of flame retardant masterbatch:

[0078] 60 parts of polyamide resin with a melt viscosity of 4500 mPa∙s and a softening point of 115℃, 20 parts of EBA resin with a butyl acrylate content of 30 wt% and a melt index of 100 g / 10 min, 10 parts of brominated epoxy resin, 10 parts of sodium antimonate, 10 parts of zinc phosphate, 10 parts of terpene resin, and 2 parts of dilauryl thiodipropionate.

[0079] The materials are mixed according to the above ratio and added to the extruder. The temperature is controlled at 235℃ and the screw speed is controlled at 55 rpm / min. After the materials are melted and mixed evenly, they are pelletized underwater to obtain flame retardant masterbatch.

[0080] (2) Flame-retardant mesh processing

[0081] Flame-retardant masterbatch is added to an extruder and reheated to melt at 245°C. The melt is then pumped through a metering pump to a spinneret. The spinneret orifice size is preferably 0.125 mm, and the number of orifices is preferably 1500. Compressed air is applied to the melt polymer to draw it into filaments. The fibers cool and solidify into a web. The preferred receiving distance for the melt-blown web is 12.5 cm, and the basis weight of the flame-retardant web is controlled at 11 g / m². 2 .

[0082] (3) Multilayer composite

[0083] A 15μm aluminum-coated 150nm ETFE film, a flame-retardant mesh film, a mesh size of 3mm, and a mesh weight of 7.5g / m² were used. 2 The polyimide-reinforced mesh is unwound sequentially, and the pressure roller is heated to 155°C with the pressure controlled at 0.32 MPa for lamination to obtain a heat-sealable, flame-retardant fluorinated composite film 4.

[0084] Example 5

[0085] (1) Preparation of flame retardant masterbatch:

[0086] 60 parts of polyamide resin with a melt viscosity of 4500 mPa∙s and a softening point of 115℃, 20 parts of EBA resin with a butyl acrylate content of 30 wt% and a melt index of 100 g / 10 min, 10 parts of brominated epoxy resin, 10 parts of sodium antimonate, 10 parts of zinc phosphate, 10 parts of petroleum resin, and 2 parts of tris(2,4-di-tert-butyl)phenyl phosphite.

[0087] The materials are mixed according to the above ratio and added to the extruder. The temperature is controlled at 220℃ and the screw speed is controlled at 40rpm / min. After the materials are melted and mixed evenly, they are pelletized underwater to obtain flame retardant masterbatch.

[0088] (2) Flame-retardant mesh processing

[0089] Flame-retardant masterbatch is added to an extruder and reheated to melt at 230°C. The melt is then pumped through a metering pump to a spinneret. The spinneret orifice size is preferably 0.1 mm, and the number of orifices is preferably 1000. Compressed air is applied to the melt polymer to draw it into filaments. The fibers cool and solidify into a web. The receiving distance for the melt-blown web is preferably 10 cm, and the basis weight of the flame-retardant web is controlled at 8 g / m². 2 .

[0090] (3) Multilayer composite

[0091] A 12μm aluminum-coated 100nm PVDF film, a flame-retardant mesh film, a mesh size of 2mm, and a mesh weight of 10g / m² are used. 2 The liquid crystal polymer reinforced mesh is unwound sequentially, the pressure roller is heated to 140°C, and the pressure is controlled at 0.25MPa for lamination to obtain a heat-sealable, flame-retardant fluorinated composite film 5.

[0092] Comparative Example 1

[0093] (1) Preparation of flame retardant masterbatch:

[0094] 90 parts of polyamide resin with a melt viscosity of 4500 mPa∙s and a softening point of 115℃, 10 parts of brominated polystyrene, 10 parts of sodium metaantimonate, 10 parts of zinc borate, and 2 parts of octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate.

[0095] The materials are mixed according to the above ratio and added to the extruder. The temperature is controlled at 250℃ and the screw speed is controlled at 70rpm / min. After the materials are melted and mixed evenly, they are granulated underwater to obtain flame retardant masterbatch.

[0096] (2) Flame-retardant mesh processing

[0097] Flame-retardant masterbatch is added to an extruder and reheated to melt at 260°C. The melt is then pumped through a metering pump to a spinneret. The spinneret orifice size is preferably 0.15 mm, and the number of orifices is preferably 2000. Compressed air is applied to the molten polymer to draw it into filaments. The fibers cool and solidify into a web. The preferred receiving distance for the melt-blown web is 15 cm, and the basis weight of the flame-retardant web is 14 g / m². 2 .

[0098] (3) Multilayer composite

[0099] A 18μm aluminum-coated 200nm PVF film, a flame-retardant mesh, a mesh size of 4mm, and a mesh weight of 5g / m² are used. 2 Nylon 66 reinforced meshes were unwound sequentially, and pressure rollers were heated to 140°C with pressure controlled at 0.4 MPa for lamination to obtain a comparative fluorinated composite film 1.

[0100] Comparative Example 2

[0101] (1) Masterbatch preparation:

[0102] 120 parts of polyamide resin with a melt viscosity of 4500 mPa∙s and a softening point of 115℃, and 2 parts of octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate.

[0103] The materials are mixed according to the above ratio and added to the extruder. The temperature is controlled at 250℃ and the screw speed is controlled at 70rpm / min. After the materials are melted and mixed evenly, they are granulated underwater to obtain flame retardant masterbatch.

[0104] (2) Membrane processing

[0105] Flame-retardant masterbatch is added to an extruder and reheated to melt at 260°C. The melt is then pumped through a metering pump to a spinneret. The spinneret orifice size is preferably 0.15 mm, and the number of orifices is preferably 2000. Compressed air is applied to the molten polymer to draw it into filaments. The fibers cool and solidify into a web. The preferred receiving distance for the melt-blown web is 15 cm, and the basis weight of the flame-retardant web is 14 g / m². 2 .

[0106] (3) Multilayer composite

[0107] A 18μm aluminum-coated 200nm PVF film, a flame-retardant mesh, a mesh size of 4mm, and a mesh weight of 5g / m² are used. 2 Nylon 66 reinforced meshes were unwound sequentially, and pressure rollers were heated to 140°C with pressure controlled at 0.4 MPa for lamination to obtain a comparative fluorinated composite film 2.

[0108] Comparative Example 3

[0109] (1) Preparation of flame retardant masterbatch:

[0110] 80 parts of polyamide resin with a melt viscosity of 4500 mPa∙s and a softening point of 115℃, 10 parts of brominated polystyrene, 10 parts of sodium metaantimonate, 10 parts of zinc borate, 10 parts of rosin resin, and 2 parts of octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate.

[0111] The materials are mixed according to the above ratio and added to the extruder. The temperature is controlled at 250℃ and the screw speed is controlled at 70rpm / min. After the materials are melted and mixed evenly, they are granulated underwater to obtain flame retardant masterbatch.

[0112] (2) Flame-retardant mesh processing

[0113] Flame-retardant masterbatch is added to an extruder and reheated to melt at 260°C. The melt is then pumped through a metering pump to a spinneret. The spinneret orifice size is preferably 0.15 mm, and the number of orifices is preferably 2000. Compressed air is applied to the molten polymer to draw it into filaments. The fibers cool and solidify into a web. The preferred receiving distance for the melt-blown web is 15 cm, and the basis weight of the flame-retardant web is 14 g / m². 2 .

[0114] (3) Multilayer composite

[0115] A 18μm aluminum-coated 200nm PVF film, a flame-retardant mesh, a mesh size of 4mm, and a mesh weight of 5g / m² are used. 2 Nylon 66 reinforced meshes were unwound sequentially, and the pressure rollers were heated to 140°C with the pressure controlled at 0.4 MPa for lamination to obtain a comparative fluorinated composite film 3.

[0116] Comparative Example 4

[0117] (1) Preparation of flame retardant masterbatch:

[0118] 60 parts of polyamide resin with a melt viscosity of 4500 mPa∙s and a softening point of 115℃, 20 parts of EBA resin with a butyl acrylate content of 30 wt% and a melt index of 100 g / 10 min, 15 parts of brominated polystyrene, 15 parts of sodium metaantimonate, 10 parts of rosin resin, and 2 parts of octadecyl β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate.

[0119] The materials are mixed according to the above ratio and added to the extruder. The temperature is controlled at 250℃ and the screw speed is controlled at 70rpm / min. After the materials are melted and mixed evenly, they are granulated underwater to obtain flame retardant masterbatch.

[0120] (2) Flame-retardant mesh processing

[0121] Flame-retardant masterbatch is added to an extruder and reheated to melt at 260°C. The melt is then pumped through a metering pump to a spinneret. The spinneret orifice size is preferably 0.15 mm, and the number of orifices is preferably 2000. Compressed air is applied to the molten polymer to draw it into filaments. The fibers cool and solidify into a web. The preferred receiving distance for the melt-blown web is 15 cm, and the basis weight of the flame-retardant web is 14 g / m². 2 .

[0122] (3) Multilayer composite

[0123] A 18μm aluminum-coated 200nm PVF film, a flame-retardant mesh, a mesh size of 4mm, and a mesh weight of 5g / m² are used. 2 Nylon 66 reinforced meshes were unwound sequentially, and the pressure rollers were heated to 140°C with the pressure controlled at 0.4 MPa for lamination to obtain a comparative fluorinated composite film 4.

[0124] The performance of the fluorinated composite membranes obtained in the examples and comparative examples was tested according to standard BMS8-377, and the results are shown in Table 1.

[0125] Table 1. Performance of fluorinated composite membranes in the examples and comparative examples.

[0126]

[0127] The above description is only a preferred embodiment of the present invention. It should be noted that for those skilled in the art, several improvements and modifications can be made without departing from the principle of the present invention, and these improvements and modifications should also be considered within the scope of protection of the present invention.

Claims

1. A heat-sealable, flame-retardant composite film, comprising an aluminized film, a flame-retardant mesh, and a reinforcing mesh sequentially laminated together; The flame-retardant mesh comprises the following components in parts by weight: 40-60 parts of polyamide resin, 10-20 parts of EBA resin, 5-10 parts of first flame retardant, 5-10 parts of second flame retardant, 5-10 parts of third flame retardant, 5-10 parts of tackifier, and 1-2 parts of antioxidant. The first flame retardant comprises brominated polystyrene and / or brominated epoxy resin; the second flame retardant comprises sodium metaantimonate and / or sodium antimonate; and the third flame retardant comprises zinc borate and / or zinc phosphate.

2. The heat-sealable, flame-retardant composite film according to claim 1, characterized in that, The polyamide resin has a melt viscosity of 2000~4500 mPa·s and a melt index of 50~100 g / 10 min.

3. The heat-sealable, flame-retardant composite film according to claim 1, characterized in that, The EBA resin contains 20-30 wt% butyl acrylate and has a melt index of 50-100 g / 10 min.

4. The heat-sealable, flame-retardant composite film according to claim 1, characterized in that, The tackifier includes one or more of rosin resin, terpene resin and petroleum resin; The antioxidants include one or more of β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate, dilauryl thiodipropionate, and tris(2,4-di-tert-butyl)phosphite.

5. The heat-sealable, flame-retardant composite film according to claim 1, characterized in that, The aluminized film includes aluminized PVF film, aluminized ETFE film, or aluminized PVDF film; The reinforcing mesh is made of one or more of nylon 66, polyimide, and liquid crystal polymer.

6. The method for preparing the heat-sealable, flame-retardant composite film as described in claim 1, comprising the following steps: A) Polyamide resin, EBA resin, first flame retardant, second flame retardant, third flame retardant, tackifier and antioxidant are melt-mixed, extruded and granulated to obtain flame retardant masterbatch; B) The flame-retardant masterbatch is melt-blown into a mesh to obtain a flame-retardant mesh film; C) The aluminum-coated film, flame-retardant mesh, and reinforcing mesh are combined to obtain a heat-sealable, flame-retardant composite film.

7. The preparation method according to claim 6, characterized in that, In step A), an extruder is used for granulation, and the temperature of the melt mixing is 220~250℃, and the screw speed is 40~70rpm.

8. The preparation method according to claim 6, characterized in that, In step B), the melt-blown web forming temperature is 230~260℃, the spinneret orifice diameter is 0.1~0.15mm, the receiving distance is 10~15cm, and the basis weight of the flame-retardant web is 8~14g / cm³. 2 .

9. The preparation method according to claim 6, characterized in that, In step C), lamination is used, and the lamination pressure is 0.25~0.4MPa and the temperature is 140~170℃.

10. The application of the heat-sealable, flame-retardant composite film as described in any one of claims 1 to 5 in aircraft thermal and sound insulation systems.

Images