A multilayer flame-retardant composite fabric for aircraft cabin based on flame-retardant fibers and a preparation method thereof

Abstract

The present application relates to the technical field of layered composite fabric, and particularly relates to a multi-layer flame-retardant composite fabric for aviation cabin based on flame-retardant fiber and a preparation method thereof.The preparation method comprises the following steps: preparing modified DOPO by reacting acrylic acid with DOPO; preparing a composite flame retardant by reacting epoxy-based POSS with the modified DOPO; preparing modified polyamide by reacting hydrophilic grafted polyamide with the composite flame retardant and amino-modified nano-montmorillonite; preparing flame-retardant fiber by melt spinning and shortening the modified polyamide; spinning the flame-retardant fiber into flame-retardant yarn, and then spinning the flame-retardant yarn into a fabric to obtain a surface fabric; mixing the flame-retardant fiber with polyester fiber to obtain blended yarn, and then spinning the blended yarn into a fabric to obtain a bottom fabric; and combining the surface fabric with the bottom fabric to obtain a composite fabric.The prepared composite fabric has excellent flame-retardant performance and anti-static performance, and can be applied to aviation cabin.

Description

Technical Field

[0001] This invention relates to the field of layered composite fabric technology, specifically to a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers and its preparation method. Background Technology

[0002] Aircraft cabin fabrics, due to their unique operating environment and safety requirements, must meet numerous stringent standards, covering aspects such as safety, functionality, durability, and aesthetics. From a safety perspective, flame retardancy is a mandatory requirement for aircraft cabin fabrics, along with antistatic properties to prevent sparks from friction that could cause hazards. For components such as seats and armrests in aircraft cabins, high-frequency use necessitates fabrics with excellent abrasion resistance. Currently, polyester and nylon are the two most commonly used materials in aircraft cabin fabrics. Nylon is more abrasion-resistant than polyester; however, nylon has flexible molecular chains and low crystallinity, while polyester has rigid molecular chains and high crystallinity. Therefore, nylon has poorer wrinkle resistance than polyester, generally requiring a composite of nylon and polyester to improve wrinkle resistance. Furthermore, improving the antistatic and flame retardant properties of nylon is necessary to enhance fabric safety.

[0003] Chinese patent application CN103287029A discloses an insulating fabric comprising a non-woven base layer and an insulating coating. The non-woven base layer is made of polyester fiber, nylon fiber, and a flame retardant. The non-woven base layer is impregnated in an insulating and flame-retardant paint to improve the fabric's insulation and flame retardancy. However, the flame-retardant components easily detach from the fabric surface, resulting in poor flame-retardant performance. Furthermore, to achieve insulation, the fabric's conductivity must be minimized. However, to achieve antistatic properties, the fabric needs a certain degree of conductivity to allow for the slow release of static charge, controlling or reducing the accumulation of surface static charge, thereby reducing the surface charge density. Summary of the Invention

[0004] To address the shortcomings of existing technologies, this invention provides a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers and its preparation method, thereby solving the problem that the flame-retardant and antistatic properties of polyamide-based fabrics in existing technologies need to be improved.

[0005] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0006] A method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers includes the following steps:

[0007] Step 1: Acrylic acid is reacted with DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) to prepare modified DOPO;

[0008] Step 2: React epoxy-based POSS (cage-type polysilsesquioxane) with modified DOPO to prepare a composite flame retardant;

[0009] Step 3: Reaction of hydrophilic grafted polyamide (PA) with composite flame retardant and amino-modified nano-montmorillonite to prepare modified polyamide;

[0010] Step 4: Modified polyamide is melt-spun, chopped, and used to obtain flame-retardant fibers;

[0011] Step 5: Spin the flame-retardant fibers into flame-retardant yarn, and then spin the flame-retardant yarn into fabric to obtain the surface fabric.

[0012] Flame-retardant fibers are blended with polyester fibers to obtain blended yarn, and then the blended yarn is spun into fabric to obtain the base fabric.

[0013] The surface fabric is combined with the bottom fabric to obtain a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers.

[0014] Preferably, step one specifically includes:

[0015] DOPO was mixed with acrylic acid and reacted. After the reaction was completed, modified DOPO was obtained.

[0016] The molar ratio of DOPO to acrylic acid is 1:1, and the reaction conditions are reflux reaction at 155-165℃ for 2.5-3.5h under a nitrogen atmosphere.

[0017] Preferably, step two specifically includes:

[0018] Epoxy POSS, polymerization inhibitor, and catalyst were added to xylene, heated to a set temperature, and modified DOPO was added. After the reaction was completed, the mixture was purified to obtain a composite flame retardant.

[0019] The molar ratio of epoxy-based POSS to modified DOPO is 1:(3-5). The reaction conditions are 6-8 hours at a set temperature of 90-110℃. The amount of xylene added is 3-5 times the mass of epoxy-based POSS. The amount of polymerization inhibitor added is 0.1%-0.3% of the total mass of epoxy-based POSS, xylene, and modified DOPO. The amount of catalyst added is 0.4%-0.8% of the total mass of epoxy-based POSS, xylene, and modified DOPO.

[0020] The epoxy group POSS includes octacyclohexyl ethyl POSS, the polymerization inhibitor includes 2,6-di-tert-butyl-p-phenol, and the catalyst includes N,N-dimethylbenzylamine.

[0021] Preferably, step three specifically includes:

[0022] Hydrophilic grafted polyamide is mixed with a composite flame retardant and amino-modified nano-montmorillonite, melted and reacted, extruded, cooled, pelletized and dried to obtain modified polyamide;

[0023] The mass ratio of hydrophilic grafted polyamide, composite flame retardant, and amino-modified nano-montmorillonite is 100:(3-5):(2-4), and the melting reaction temperature is 270-290℃.

[0024] Preferably, the amino-modified nano-montmorillonite is prepared by the following steps:

[0025] Add γ-aminopropyltriethoxysilane (silane coupling agent KH-550) to an aqueous ethanol solution and adjust the pH to 3.5-4.5 to obtain a γ-aminopropyltriethoxysilane solution.

[0026] A solution of γ-aminopropyltriethoxysilane was added dropwise to a nano-montmorillonite dispersion, and the reaction was carried out. After the reaction was completed, the mixture was purified and dried to obtain amino-modified nano-montmorillonite.

[0027] The mass ratio of nano-montmorillonite dispersion, γ-aminopropyltriethoxysilane, and aqueous ethanol solution is 50:(0.5-1.5):(10-20), and the reaction conditions are 3.5-4.5 h at 55-65℃.

[0028] Preferably, the ethanol aqueous solution comprises a 95wt% ethanol aqueous solution; the nano-montmorillonite dispersion is prepared by nano-montmorillonite and chloroform, and the mass percentage of nano-montmorillonite in the nano-montmorillonite dispersion is 5%-9%.

[0029] Preferably, the hydrophilic grafted polyamide is prepared by the following steps:

[0030] Polyamide resin powder was added to potassium persulfate aqueous solution and a pre-initiation reaction was carried out under stirring. After the reaction was completed, the mixture was filtered and dried to obtain pre-initiated polyamide resin powder.

[0031] The mass ratio of polyamide resin powder to potassium persulfate aqueous solution is 1:(20-30), the reaction conditions are 70-80℃ for 1-2 hours, and the potassium persulfate aqueous solution is 0.5wt% potassium persulfate aqueous solution.

[0032] The pre-initiated polyamide resin powder was added to the hydrophilic monomer solution, and the reaction was carried out. After the reaction was completed, the mixture was filtered, washed, and dried to obtain the hydrophilic grafted polyamide.

[0033] The mass ratio of pre-initiated polyamide resin powder to hydrophilic monomer solution is 1:(30-50). The reaction conditions are 70-90℃ for 1.5-2.5h. The hydrophilic monomer solution is prepared by hydrophilic monomers 2-acrylamide-2-methylpropanesulfonic acid, hydroxyethyl methacrylate, and deionized water. The molar ratio of 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate is 1:1. The total amount of 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate in the hydrophilic monomer solution is 20wt%.

[0034] Preferably, in step four, the process parameters for melt spinning include: a melt temperature of 280-300℃, 15-30 holes in the spinneret with a hole diameter of 0.1-0.2mm, a winding speed of 300-500 meters / minute, and a winding temperature of 18-19℃.

[0035] The obtained flame-retardant fiber monofilament fineness is 0.8-3 dtex.

[0036] Preferably, in step five, the flame-retardant yarn has a yarn count of 8-50S (English count) and the surface fabric has a weight of 100-500 g / m². 2 .

[0037] Preferably, in step five, the mass ratio of flame-retardant fiber to polyester fiber is 1:(1-3), the yarn count of the blended yarn is 8-50S, and the weight of the base fabric is 100-500g / m². 2 .

[0038] A multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers, prepared by the method described above.

[0039] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0040] The multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers of the present invention includes a top layer fabric and a bottom layer fabric. The top layer fabric is made of polyamide fiber, which has good abrasion resistance and small single filament fineness, belonging to ultrafine fiber. The resulting top layer fabric has a soft and flexible feel. The bottom layer fabric is made of a blend of polyamide fiber and polyester fiber, which has good wrinkle resistance. When combined with the top layer fabric, the resulting composite fabric has good wrinkle resistance.

[0041] The polyamide fiber in this invention is a flame-retardant material obtained by melt spinning after modification of polyamide. The composite flame retardant is made from POSS and DOPO. POSS, as a nano flame retardant, can significantly improve the flame retardant performance of the material through the synergistic effect of multiple mechanisms such as physical barrier, free radical capture, and char layer enhancement. DOPO decomposes at high temperature to generate phosphorus-containing free radicals, which can capture H· and OH· free radicals in the combustion chain reaction and inhibit flame propagation. At the same time, after decomposition, it forms phosphoric acid or polyphosphoric acid, which promotes char formation on the material surface and forms a heat-insulating and oxygen-barrier char layer, slowing down pyrolysis and the release of combustible gases. The synergistic effect of POSS and DOPO results in good flame retardant effect. DOPO undergoes a nucleophilic addition reaction with the carbon-carbon double bond in the acrylic acid molecule through a highly reactive PH bond, and then undergoes a ring-opening reaction with the epoxy group in the epoxy group of the POSS molecule through the introduced carboxyl group, thus realizing the chemical bonding between POSS and DOPO.

[0042] In this invention, the introduction of nano-montmorillonite during the preparation of modified polyamide can improve the flame retardant and antistatic properties of polyamide. After amino modification, the nano-montmorillonite can react with the epoxy groups on the epoxy group POSS molecule during the melt reaction with polyamide and composite flame retardant, thus linking the nano-montmorillonite to the composite flame retardant molecule with stable chemical bonds.

[0043] The polyamide in this invention undergoes hydrophilic grafting modification, introducing hydrophilic hydroxyl and carboxyl groups. This not only enhances the hydrophilicity of the polyamide, enabling it to absorb environmental moisture and form a conductive surface layer, thus improving its antistatic properties, but also allows the hydroxyl and carboxyl groups to react with the epoxy groups on the POSS molecules in the composite flame retardant, thereby connecting the composite flame retardant to the polyamide molecule. This results in good compatibility and dispersion uniformity between the composite flame retardant and the polyamide, and excellent flame retardant performance of the polyamide. Attached Figure Description

[0044] Figure 1 This is a schematic diagram illustrating the reaction of DOPO with acrylic acid to prepare modified DOPO in Example 1 of the present invention;

[0045] Figure 2 This is a schematic diagram illustrating the preparation of a composite flame retardant by reacting modified DOPO with octacyclooxycyclohexylethyl POSS in Example 1 of the present invention.

[0046] Figure 3 The infrared spectrum of the modified DOPO prepared in Example 1 of this invention;

[0047] Figure 4 Line graphs showing the flame retardant performance test results of the surface fabrics prepared in Examples 1-5 and Comparative Examples 1-2 of the present invention.

[0048] Figure 5Line graphs showing the antistatic performance test results of the surface fabrics prepared in Examples 1-5 and Comparative Examples 1-2 of the present invention. Detailed Implementation

[0049] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0050] Example 1

[0051] This embodiment discloses a method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers, including the following steps:

[0052] Step 1: Mix DOPO with acrylic acid at a molar ratio of 1:1. Reflux the mixture at 155°C for 3.5 hours under a nitrogen atmosphere. After the reaction is complete, cool to room temperature to obtain modified DOPO.

[0053] Depend on Figure 3 It can be known that 3440cm -1 The peak at 2920 cm⁻¹ is the characteristic absorption peak of the OH group in the acrylic acid molecule. -1 The characteristic absorption peak of -CH2- is at 1705 cm⁻¹. -1 The peak at 1425 cm⁻¹ is the characteristic absorption peak of the C=O group on the carboxylic acid group. -1 The characteristic absorption peak of PC is at 1180 cm⁻¹. -1 The characteristic absorption peak at point P=O is located there.

[0054] Step 2: Add octacyclohexyl ethyl POSS, 2,6-di-tert-butyl-p-phenol, and N,N-dimethylbenzylamine to xylene, heat to 90°C, add modified DOPO, and react at 90°C for 8 hours. After the reaction is complete, cool to room temperature, pour off the upper layer solution, add acetone (3 times the mass of the lower layer reactants) to the lower layer reactants for washing, and remove the acetone by vacuum distillation to obtain the composite flame retardant.

[0055] The molar ratio of epoxy POSS to modified DOPO is 1:3; the amount of xylene added is 3 times the mass of epoxy POSS; the amount of 2,6-di-tert-butyl-p-phenol added is 0.1% of the total mass of epoxy POSS, xylene, and modified DOPO; and the amount of N,N-dimethylbenzylamine added is 0.4% of the total mass of epoxy POSS, xylene, and modified DOPO.

[0056] Step 3: Mix hydrophilic grafted PA66 with composite flame retardant and amino-modified nano-montmorillonite. The mass ratio of hydrophilic grafted PA66 to composite flame retardant and amino-modified nano-montmorillonite is 100:3:2. Melt reaction is carried out at a temperature of 270℃. Extrusion, cooling, pelletizing and drying are performed to obtain modified polyamide.

[0057] The amino-modified nano-montmorillonite is prepared by the following steps:

[0058] Add γ-aminopropyltriethoxysilane to a 95wt% aqueous ethanol solution and adjust the pH to 4 to obtain a γ-aminopropyltriethoxysilane solution.

[0059] A solution of γ-aminopropyltriethoxysilane was added dropwise to a nano-montmorillonite dispersion and reacted at 60°C for 4 hours. After the reaction was completed, the mixture was filtered, washed three times with ethanol, and then dried in a vacuum drying oven at 50°C to constant weight to obtain amino-modified nano-montmorillonite.

[0060] The mass ratio of nano-montmorillonite dispersion, γ-aminopropyltriethoxysilane, and 95wt% ethanol aqueous solution is 50:0.5:10. The nano-montmorillonite dispersion is prepared by mixing nano-montmorillonite and chloroform, and the mass percentage of nano-montmorillonite in the nano-montmorillonite dispersion is 8%.

[0061] The hydrophilic grafted PA66 is prepared by the following steps:

[0062] PA66 powder was added to a 0.5wt% potassium persulfate aqueous solution at a mass ratio of 1:25. The pre-initiation reaction was carried out under stirring at 300 r / min and at 75℃ for 1.5 h. After the reaction was completed, the mixture was filtered and dried in a vacuum drying oven at 50℃ until constant weight to obtain the pre-initiated PA66 powder.

[0063] The pre-initiated PA66 powder was added to the hydrophilic monomer solution at a mass ratio of 1:40. The reaction was carried out at 80℃ for 2 hours. After the reaction was completed, the mixture was filtered, washed three times with deionized water, and dried in a vacuum drying oven at 50℃ until constant weight to obtain hydrophilic grafted polyamide.

[0064] The hydrophilic monomer solution is prepared by hydrophilic monomers 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate with deionized water. The molar ratio of 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate is 1:1, and the total amount of 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate in the hydrophilic monomer solution is 20 wt%.

[0065] Step 4: Modified polyamide melt spinning. The process parameters for melt spinning include: melt temperature of 280℃, spinneret with 25 holes and a hole diameter of 0.15mm, winding speed of 400m / min, winding temperature of 18℃, and chopped short to obtain flame-retardant fibers.

[0066] The flame-retardant fiber monofilament fineness is 1.5 dtex, and the flame-retardant fiber length is 38-51 mm;

[0067] Step 5: Spin the flame-retardant fibers into flame-retardant yarn with a yarn count of 40S. Then spin the flame-retardant yarn into fabric to obtain the surface fabric, which has a weight of 200g / m². 2 ;

[0068] Flame-retardant fiber is blended with polyester fiber at a mass ratio of 1:1 to obtain a blended yarn with a yarn count of 40S. This blended yarn is then spun into a base fabric with a weight of 200 g / m². 2 ;

[0069] The surface fabric and the bottom fabric are sewn together using polyester sewing thread and other materials to obtain a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers.

[0070] Example 2

[0071] This embodiment discloses a method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers, including the following steps:

[0072] Step 1: Mix DOPO with acrylic acid at a molar ratio of 1:1. Reflux the mixture at 165°C for 2.5 hours under a nitrogen atmosphere. After the reaction is complete, cool to room temperature to obtain modified DOPO.

[0073] Step 2: Add octacyclohexyl ethyl POSS, 2,6-di-tert-butyl-p-phenol, and N,N-dimethylbenzylamine to xylene, heat to 110°C, add modified DOPO, and react at 110°C for 6 hours. After the reaction is complete, cool to room temperature, pour off the upper layer solution, add acetone (3 times the mass of the lower layer reactants) to the lower layer reactants for washing, and remove the acetone by vacuum distillation to obtain the composite flame retardant.

[0074] The molar ratio of epoxy POSS to modified DOPO is 1:5, the amount of xylene added is 5 times the mass of epoxy POSS, the amount of 2,6-di-tert-butyl-p-phenol added is 0.3% of the total mass of epoxy POSS, xylene, and modified DOPO, and the amount of N,N-dimethylbenzylamine added is 0.8% of the total mass of epoxy POSS, xylene, and modified DOPO.

[0075] Step 3: Mix hydrophilic grafted PA66 with composite flame retardant and amino-modified nano-montmorillonite. The mass ratio of hydrophilic grafted PA66 to composite flame retardant and amino-modified nano-montmorillonite is 100:5:4. Melt reaction is carried out at a temperature of 290℃. Extrusion, cooling, pelletizing and drying are performed to obtain modified polyamide.

[0076] The preparation methods of the amino-modified nano-montmorillonite and the hydrophilic grafted PA66 are the same as in Example 1;

[0077] Step 4: Modified polyamide melt spinning. The process parameters for melt spinning include: melt temperature of 300℃, spinneret with 25 holes and a hole diameter of 0.15mm, winding speed of 400m / min, winding temperature of 18℃, and chopped short to obtain flame-retardant fibers.

[0078] The flame-retardant fiber monofilament fineness is 1.5 dtex, and the flame-retardant fiber length is 38-51 mm;

[0079] Step 5: Spin the flame-retardant fibers into flame-retardant yarn with a yarn count of 40S. Then spin the flame-retardant yarn into fabric to obtain the surface fabric, which has a weight of 200g / m². 2 ;

[0080] Flame-retardant fiber is blended with polyester fiber at a mass ratio of 1:3 to obtain a blended yarn with a yarn count of 40S. This blended yarn is then spun into a base fabric with a weight of 200 g / m². 2 ;

[0081] The surface fabric and the bottom fabric are sewn together using polyester sewing thread and other materials to obtain a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers.

[0082] Example 3

[0083] This embodiment discloses a method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers, including the following steps:

[0084] Step 1: Mix DOPO with acrylic acid at a molar ratio of 1:1. Reflux the mixture at 160°C for 3 hours under a nitrogen atmosphere. After the reaction is complete, cool to room temperature to obtain modified DOPO.

[0085] Step 2: Add octacyclohexyl ethyl POSS, 2,6-di-tert-butyl-p-phenol, and N,N-dimethylbenzylamine to xylene, heat to 100°C, add modified DOPO, and react at 100°C for 7 hours. After the reaction is complete, cool to room temperature, pour off the upper layer solution, add acetone (3 times the mass of the lower layer reactants) to the lower layer reactants for washing, and remove the acetone by vacuum distillation to obtain the composite flame retardant.

[0086] The molar ratio of epoxy POSS to modified DOPO is 1:4; the amount of xylene added is 4 times the mass of epoxy POSS; the amount of 2,6-di-tert-butyl-p-phenol added is 0.15% of the total mass of epoxy POSS, xylene, and modified DOPO; and the amount of N,N-dimethylbenzylamine added is 0.5% of the total mass of epoxy POSS, xylene, and modified DOPO.

[0087] Step 3: Mix hydrophilic grafted PA66 with composite flame retardant and amino-modified nano-montmorillonite. The mass ratio of hydrophilic grafted PA66 to composite flame retardant and amino-modified nano-montmorillonite is 100:3.5:2.5. Melt reaction is carried out at a temperature of 280℃. Extrusion, cooling, pelletizing and drying are performed to obtain modified polyamide.

[0088] The preparation methods of the amino-modified nano-montmorillonite and the hydrophilic grafted PA66 are the same as in Example 1;

[0089] Step 4: Modified polyamide melt spinning. The process parameters for melt spinning include: melt temperature of 290℃, spinneret with 25 holes and a hole diameter of 0.15mm, winding speed of 400m / min, winding temperature of 18℃, and chopped short to obtain flame-retardant fibers.

[0090] The flame-retardant fiber monofilament fineness is 1.5 dtex, and the flame-retardant fiber length is 38-51 mm;

[0091] Step 5: Spin the flame-retardant fibers into flame-retardant yarn with a yarn count of 40S. Then spin the flame-retardant yarn into fabric to obtain the surface fabric, which has a weight of 200g / m². 2 ;

[0092] Flame-retardant fiber is blended with polyester fiber at a mass ratio of 1:1.5 to obtain a blended yarn with a yarn count of 40S. This blended yarn is then spun into a base fabric with a weight of 200 g / m². 2 ;

[0093] The surface fabric and the bottom fabric are sewn together using polyester sewing thread and other materials to obtain a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers.

[0094] Example 4

[0095] This embodiment discloses a method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers, including the following steps:

[0096] Step 1: Mix DOPO with acrylic acid at a molar ratio of 1:1. Reflux the mixture at 160°C for 3 hours under a nitrogen atmosphere. After the reaction is complete, cool to room temperature to obtain modified DOPO.

[0097] Step 2: Add octacyclohexyl ethyl POSS, 2,6-di-tert-butyl-p-phenol, and N,N-dimethylbenzylamine to xylene, heat to 100°C, add modified DOPO, and react at 100°C for 7 hours. After the reaction is complete, cool to room temperature, pour off the upper layer solution, add acetone (3 times the mass of the lower layer reactants) to the lower layer reactants for washing, and remove the acetone by vacuum distillation to obtain the composite flame retardant.

[0098] The molar ratio of epoxy POSS to modified DOPO is 1:4, the amount of xylene added is 4 times the mass of epoxy POSS, the amount of 2,6-di-tert-butyl-p-phenol added is 0.2% of the total mass of epoxy POSS, xylene, and modified DOPO, and the amount of N,N-dimethylbenzylamine added is 0.6% of the total mass of epoxy POSS, xylene, and modified DOPO.

[0099] Step 3: Mix hydrophilic grafted PA66 with composite flame retardant and amino-modified nano-montmorillonite. The mass ratio of hydrophilic grafted PA66 to composite flame retardant and amino-modified nano-montmorillonite is 100:4:3. Melt reaction is carried out at a temperature of 280℃. Extrusion, cooling, pelletizing and drying are performed to obtain modified polyamide.

[0100] The preparation methods of the amino-modified nano-montmorillonite and the hydrophilic grafted PA66 are the same as in Example 1;

[0101] Step 4: Modified polyamide melt spinning. The process parameters for melt spinning include: melt temperature of 290℃, spinneret with 25 holes and a hole diameter of 0.15mm, winding speed of 400m / min, winding temperature of 18℃, and chopped short to obtain flame-retardant fibers.

[0102] The flame-retardant fiber monofilament fineness is 1.5 dtex, and the flame-retardant fiber length is 38-51 mm;

[0103] Step 5: Spin the flame-retardant fibers into flame-retardant yarn with a yarn count of 40S. Then spin the flame-retardant yarn into fabric to obtain the surface fabric, which has a weight of 200g / m². 2 ;

[0104] Flame-retardant fiber is blended with polyester fiber at a mass ratio of 1:2 to obtain a blended yarn with a yarn count of 40S. This blended yarn is then spun into a base fabric with a weight of 200 g / m². 2 ;

[0105] The surface fabric and the bottom fabric are sewn together using polyester sewing thread and other materials to obtain a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers.

[0106] Example 5

[0107] This embodiment discloses a method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers, including the following steps:

[0108] Step 1: Mix DOPO with acrylic acid at a molar ratio of 1:1. Reflux the mixture at 160°C for 3 hours under a nitrogen atmosphere. After the reaction is complete, cool to room temperature to obtain modified DOPO.

[0109] Step 2: Add octacyclohexyl ethyl POSS, 2,6-di-tert-butyl-p-phenol, and N,N-dimethylbenzylamine to xylene, heat to 100°C, add modified DOPO, and react at 100°C for 7 hours. After the reaction is complete, cool to room temperature, pour off the upper layer solution, add acetone (3 times the mass of the lower layer reactants) to the lower layer reactants for washing, and remove the acetone by vacuum distillation to obtain the composite flame retardant.

[0110] The molar ratio of epoxy POSS to modified DOPO is 1:4, the amount of xylene added is 4 times the mass of epoxy POSS, the amount of 2,6-di-tert-butyl-p-phenol added is 0.25% of the total mass of epoxy POSS, xylene, and modified DOPO, and the amount of N,N-dimethylbenzylamine added is 0.7% of the total mass of epoxy POSS, xylene, and modified DOPO.

[0111] Step 3: Mix hydrophilic grafted PA66 with composite flame retardant and amino-modified nano-montmorillonite. The mass ratio of hydrophilic grafted PA66 to composite flame retardant and amino-modified nano-montmorillonite is 100:4.5:3.5. Melt reaction is carried out at a temperature of 280℃. Extrusion, cooling, pelletizing and drying are performed to obtain modified polyamide.

[0112] The preparation methods of the amino-modified nano-montmorillonite and the hydrophilic grafted PA66 are the same as in Example 1;

[0113] Step 4: Modified polyamide melt spinning. The process parameters for melt spinning include: melt temperature of 290℃, spinneret with 25 holes and a hole diameter of 0.15mm, winding speed of 400m / min, winding temperature of 18℃, and chopped short to obtain flame-retardant fibers.

[0114] The flame-retardant fiber monofilament fineness is 1.5 dtex, and the flame-retardant fiber length is 38-51 mm;

[0115] Step 5: Spin the flame-retardant fibers into flame-retardant yarn with a yarn count of 40S. Then spin the flame-retardant yarn into fabric to obtain the surface fabric, which has a weight of 200g / m². 2 ;

[0116] Flame-retardant fiber is blended with polyester fiber at a mass ratio of 1:2.5 to obtain a blended yarn with a yarn count of 40S. This blended yarn is then spun into a base fabric with a weight of 200 g / m². 2 ;

[0117] The surface fabric and the bottom fabric are sewn together using polyester sewing thread and other materials to obtain a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers.

[0118] Comparative Example 1

[0119] This comparative example discloses a method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers, including the following steps:

[0120] Step 1: Mix DOPO with acrylic acid at a molar ratio of 1:1. Reflux the mixture at 155°C for 3.5 hours under a nitrogen atmosphere. After the reaction is complete, cool to room temperature to obtain modified DOPO.

[0121] Step 2: Add octacyclohexyl ethyl POSS, 2,6-di-tert-butyl-p-phenol, and N,N-dimethylbenzylamine to xylene, heat to 90°C, add modified DOPO, and react at 90°C for 8 hours. After the reaction is complete, cool to room temperature, pour off the upper layer solution, add acetone (3 times the mass of the lower layer reactants) to the lower layer reactants for washing, and remove the acetone by vacuum distillation to obtain the composite flame retardant.

[0122] The molar ratio of epoxy POSS to modified DOPO is 1:3; the amount of xylene added is 3 times the mass of epoxy POSS; the amount of 2,6-di-tert-butyl-p-phenol added is 0.1% of the total mass of epoxy POSS, xylene, and modified DOPO; and the amount of N,N-dimethylbenzylamine added is 0.4% of the total mass of epoxy POSS, xylene, and modified DOPO.

[0123] Step 3: PA66 powder is mixed with composite flame retardant and amino-modified nano-montmorillonite. The mass ratio of PA66 powder to composite flame retardant and amino-modified nano-montmorillonite is 100:3:2. The mixture is melted and reacted at a temperature of 270℃. The mixture is then extruded, cooled, pelletized, and dried to obtain modified polyamide.

[0124] The preparation method of the amino-modified nano-montmorillonite is the same as in Example 1;

[0125] Step 4: Modified polyamide melt spinning. The process parameters for melt spinning include: melt temperature of 280℃, spinneret with 25 holes and a hole diameter of 0.15mm, winding speed of 400m / min, winding temperature of 18℃, and chopped short to obtain flame-retardant fibers.

[0126] The flame-retardant fiber monofilament fineness is 1.5 dtex, and the flame-retardant fiber length is 38-51 mm;

[0127] Step 5: Spin the flame-retardant fibers into flame-retardant yarn with a yarn count of 40S. Then spin the flame-retardant yarn into fabric to obtain the surface fabric, which has a weight of 200g / m². 2 ;

[0128] Flame-retardant fiber is blended with polyester fiber at a mass ratio of 1:1 to obtain a blended yarn with a yarn count of 40S. This blended yarn is then spun into a base fabric with a weight of 200 g / m². 2 ;

[0129] The surface fabric and the bottom fabric are sewn together using polyester sewing thread and other materials to obtain a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers.

[0130] Comparative Example 2

[0131] This comparative example discloses a method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers, including the following steps:

[0132] Step 1: PA66 powder is mixed with DOPO, octacyclooxycyclohexylethyl POSS, and nano-montmorillonite. The mass ratio of PA66 powder, DOPO, octacyclooxycyclohexylethyl POSS, and nano-montmorillonite is 100.4:1.9:0.9:1.8. The mixture is melted at 270℃, extruded, cooled, pelletized, and dried to obtain modified polyamide.

[0133] Step 2: Modified polyamide melt spinning. The process parameters for melt spinning include: melt temperature of 280℃, spinneret with 25 holes and a hole diameter of 0.15mm, winding speed of 400m / min, winding temperature of 18℃, and chopped short to obtain flame-retardant fibers.

[0134] The flame-retardant fiber monofilament fineness is 1.5 dtex, and the flame-retardant fiber length is 38-51 mm;

[0135] Step 3: Spin the flame-retardant fibers into flame-retardant yarn with a yarn count of 40S. Then spin the flame-retardant yarn into fabric to obtain the surface fabric, which has a weight of 200g / m². 2 ;

[0136] Flame-retardant fiber is blended with polyester fiber at a mass ratio of 1:1 to obtain a blended yarn with a yarn count of 40S. This blended yarn is then spun into a base fabric with a weight of 200 g / m². 2 ;

[0137] The surface fabric and the bottom fabric are sewn together using polyester sewing thread and other materials to obtain a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers.

[0138] In the above examples and comparative examples, nano-montmorillonite was purchased from Guangzhou Yifeng Chemical Technology Co., Ltd., model: TY-710C, particle size: 50nm; PA66 powder was purchased from Dongguan Weicai Plastic Raw Materials Co., Ltd., specification: 200 mesh, melting temperature: 255℃; polyester fiber was purchased from Shandong Oude Chemical Fiber Products Co., Ltd., monofilament fineness: 0.5D, length: 4mm; polyester sewing thread was purchased from Yiwu Shenkai Thread Industry Co., Ltd., specification: 40S / 2.

[0139] Test case

[0140] (1) Flame retardant performance: The surface fabrics prepared in Examples 1-5 and Comparative Examples 1-2 were cut into samples of 150mm×58mm, and the limiting oxygen index of the samples was determined: The samples were placed in a glass bucket supported by a rectangular frame. When the surrounding oxygen concentration reached a stable level, the samples were ignited from the top. The flame height of the igniter was about 20mm. The fabric was ignited from top to bottom. When the burning time of the fabric was less than 30s, the oxygen concentration was the critical oxygen concentration required for the fabric to burn, i.e., the limiting oxygen index. The surface fabrics prepared in Examples 1-5 and Comparative Examples 1-2 were cut into samples of 300mm×80mm, and the damage length of the samples was determined: The samples were clamped with a rectangular sample clamp and suspended vertically in the reaction chamber. A layer of degreased cotton was placed underneath. The ignition time was selected as 12s, the flame height was controlled as 40mm, and the damage length during combustion was recorded. The results are shown in Table 1.

[0141] Table 1

[0142]

[0143] As shown in Table 1, the surface fabric prepared by this invention has good flame retardant properties, thereby improving the flame retardant properties of the composite fabric. Using POSS and DOPO as flame retardant components, they work synergistically, resulting in good flame retardant effect. Furthermore, POSS and DOPO are linked by stable chemical bonds and then incorporated into the polyamide molecule, resulting in good compatibility and dispersion uniformity between the composite flame retardant and the polyamide, leading to good flame retardant properties of the polyamide. The introduction of nano-montmorillonite further enhances the flame retardant properties. Compared to Example 1, in Comparative Example 1, the polyamide was not hydrophilically grafted, meaning no hydrophilic groups were introduced. The composite flame retardant could only bond with the amine and carboxyl groups located at the ends of the polyamide molecule, reducing the compatibility and dispersion uniformity between the composite flame retardant and nano-montmorillonite and the polyamide, thus decreasing the flame retardant properties. Compared to Comparative Example 1, in Comparative Example 2, POSS, DOPO, and nano-montmorillonite did not bond, meaning only POSS could bond with the amine and carboxyl groups at the ends of the polyamide molecule through epoxy groups, further reducing the flame retardant properties.

[0144] (2) Antistatic properties: The surface charge density of the surface fabrics prepared in Examples 1-5 and Comparative Examples 1-2 was determined according to the standard GB / T12703.2-2009 "Evaluation of electrostatic properties of textiles - Part 2: Surface charge density". The results are shown in Table 2.

[0145] Table 2

[0146]

[0147] As shown in Table 2, the surface fabric prepared by this invention has good antistatic properties. The polyamide undergoes hydrophilic grafting modification, introducing hydrophilic hydroxyl and carboxyl groups, which improves its antistatic properties. The introduction of nano-montmorillonite further enhances the antistatic properties of the polyamide. Compared to Example 1, in Comparative Example 1, the polyamide was not hydrophilic grafted, and the bonding amount between nano-montmorillonite and polyamide was reduced, resulting in a significant decrease in antistatic properties. Compared to Comparative Example 1, in Comparative Example 2, the compatibility and dispersion uniformity between nano-montmorillonite and polyamide further decreased, leading to a further decrease in antistatic properties.

[0148] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers, characterized in that, Includes the following steps: Step 1: React acrylic acid with DOPO to prepare modified DOPO; The molar ratio of DOPO to acrylic acid is 1:

1. Step 2: React epoxy group POSS with modified DOPO to prepare a composite flame retardant; The molar ratio of epoxy-based POSS to modified DOPO is 1:(3-5); Step 3: The hydrophilic grafted polyamide is mixed with the composite flame retardant and amino-modified nano-montmorillonite, melted and reacted, extruded, cooled, pelletized and dried to obtain the modified polyamide; The mass ratio of hydrophilic grafted polyamide, composite flame retardant, and amino-modified nano-montmorillonite is 100:(3-5):(2-4), and the melting reaction temperature is 270-290℃. The hydrophilic grafted polyamide is prepared by the following steps: Polyamide resin powder was added to potassium persulfate aqueous solution and a pre-initiation reaction was carried out under stirring. After the reaction was completed, the mixture was filtered and dried to obtain pre-initiated polyamide resin powder. The mass ratio of polyamide resin powder to potassium persulfate aqueous solution is 1:(20-30), the reaction conditions are 70-80℃ for 1-2 hours, and the potassium persulfate aqueous solution is 0.5wt% potassium persulfate aqueous solution. The pre-initiated polyamide resin powder was added to the hydrophilic monomer solution, and the reaction was carried out. After the reaction was completed, the mixture was filtered, washed, and dried to obtain the hydrophilic grafted polyamide. The mass ratio of pre-initiated polyamide resin powder to hydrophilic monomer solution is 1:(30-50). The reaction conditions are 70-90℃ for 1.5-2.5h. The hydrophilic monomer solution is prepared by hydrophilic monomers 2-acrylamide-2-methylpropanesulfonic acid, hydroxyethyl methacrylate, and deionized water. The molar ratio of 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate is 1:

1. The total amount of 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate in the hydrophilic monomer solution is 20wt%. Step 4: Modified polyamide is melt-spun, chopped, and used to obtain flame-retardant fibers; Step 5: Spin the flame-retardant fibers into flame-retardant yarn, and then spin the flame-retardant yarn into fabric to obtain the surface fabric. Flame-retardant fibers are blended with polyester fibers to obtain blended yarn, and then the blended yarn is spun into fabric to obtain the base fabric. The surface fabric is combined with the bottom fabric to obtain a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers.

2. The method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers according to claim 1, characterized in that, Step one specifically includes: DOPO was mixed with acrylic acid and reacted. After the reaction was completed, modified DOPO was obtained. The reaction conditions were as follows: reflux reaction at 155-165℃ for 2.5-3.5 hours under a nitrogen atmosphere.

3. The method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers according to claim 1, characterized in that, Step two specifically includes: Epoxy POSS, polymerization inhibitor, and catalyst were added to xylene, heated to a set temperature, and modified DOPO was added. After the reaction was completed, the mixture was purified to obtain a composite flame retardant. The reaction conditions are as follows: reaction time is 6-8 hours at a set temperature of 90-110℃; the amount of xylene added is 3-5 times the mass of epoxy-based POSS; the amount of polymerization inhibitor added is 0.1%-0.3% of the total mass of epoxy-based POSS, xylene, and modified DOPO; and the amount of catalyst added is 0.4%-0.8% of the total mass of epoxy-based POSS, xylene, and modified DOPO. The epoxy group POSS includes octacyclohexyl ethyl POSS, the polymerization inhibitor includes 2,6-di-tert-butyl-p-phenol, and the catalyst includes N,N-dimethylbenzylamine.

4. The method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers according to claim 1, characterized in that, The amino-modified nano-montmorillonite is prepared by the following steps: Add γ-aminopropyltriethoxysilane to an aqueous ethanol solution and adjust the pH to 3.5-4.5 to obtain a γ-aminopropyltriethoxysilane solution. A solution of γ-aminopropyltriethoxysilane was added dropwise to a nano-montmorillonite dispersion, and the reaction was carried out. After the reaction was completed, the mixture was purified and dried to obtain amino-modified nano-montmorillonite. The mass ratio of nano-montmorillonite dispersion, γ-aminopropyltriethoxysilane, and aqueous ethanol solution is 50:(0.5-1.5):(10-20), and the reaction conditions are 3.5-4.5 h at 55-65℃.

5. The method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers according to claim 1, characterized in that, In step four, the process parameters for melt spinning include: a melt temperature of 280-300℃, 15-30 holes in the spinneret, a hole diameter of 0.1-0.2mm, a winding speed of 300-500 meters / minute, and a winding temperature of 18-19℃. The obtained flame-retardant fiber monofilament fineness is 0.8-3 dtex.

6. The method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers according to claim 1, characterized in that, In step five, the flame-retardant yarn has a yarn count of 8-50S, and the surface fabric has a weight of 100-500 g / m². 2 .

7. The method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers according to claim 1, characterized in that, In step five, the mass ratio of flame-retardant fiber to polyester fiber is 1:(1-3), the yarn count of the blended yarn is 8-50S, and the weight of the base fabric is 100-500g / m². 2 .

8. A multi-layer flame-retardant composite fabric for aircraft cabin based on flame-retardant fibers, prepared by the preparation method of the multi-layer flame-retardant composite fabric for aircraft cabin based on flame-retardant fibers as described in any one of claims 1-7.

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