Flame-retardant-fiber-based multilayer flame-retardant composite fabric for aircraft cabin and preparation method of flame-retardant-fiber-based multilayer flame-retardant composite fabric

Abstract

The invention relates to the technical field of layered composite fabrics, in particular to a flame-retardant-fiber-based multilayer flame-retardant composite fabric for an aircraft cabin and a preparation method of the flame-retardant-fiber-based multilayer flame-retardant composite fabric. The preparation method comprises the following steps: reacting acrylic acid with DOPO to prepare modified DOPO; reacting the epoxy POSS with the modified DOPO to prepare a composite flame retardant; reacting the hydrophilic grafted polyamide with a composite flame retardant and amino-modified nano-montmorillonite to prepare modified polyamide; carrying out melt spinning and chopping on the modified polyamide to obtain flame-retardant fibers; the flame-retardant fibers are spun into flame-retardant yarns, then the flame-retardant yarns are spun into a fabric, and a surface fabric is obtained; the flame-retardant fibers and the polyester fibers are blended to obtain blended yarns, and then the blended yarns are spun into a fabric to obtain a bottom layer fabric; and compounding the surface layer fabric and the bottom layer fabric to obtain the composite fabric. The prepared composite fabric has excellent flame retardant property and antistatic property, and can be applied to aviation cabins.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of layered composite fabric, in particular to a multi-layer flame-retardant composite fabric for aircraft cabin based on flame-retardant fiber and a preparation method thereof. BACKGROUND

[0002] The fabric for aircraft cabin needs to meet a number of strict standards, including safety, functionality, durability and aesthetics, due to its special use environment and safety requirements. From the perspective of safety, flame-retardant performance is a requirement that the fabric for aircraft cabin must have, and it also needs to have antistatic performance to avoid friction sparks that can cause danger. For the seats, armrests and other parts of the aircraft cabin, the fabric needs to have good wear resistance due to high frequency of use. At present, polyester (polyester) and nylon (polyamide) are the two most commonly used materials in aircraft cabin fabric. Nylon is more wear-resistant than polyester, but nylon has a flexible molecular chain and low crystallinity, while polyester has a rigid molecular chain and high crystallinity, so the anti-wrinkle performance of nylon is poorer than that of polyester. Therefore, it is necessary to combine nylon with polyester to improve the anti-wrinkle performance of the fabric. In addition, the antistatic performance and flame-retardant performance of nylon need to be improved to improve the safety of the fabric.

[0003] Chinese patent application CN103287029A discloses an insulating fabric, which comprises a non-woven fabric base layer and an insulating coating. The raw material of the non-woven fabric base layer is polyester fiber, nylon fiber and flame retardant. The non-woven fabric base layer is immersed in an insulating flame-retardant paint to improve the insulating and flame-retardant properties of the fabric. However, the flame-retardant components are prone to fall off from the surface of the fabric, resulting in poor flame-retardant performance. In addition, in order to achieve the insulating property of the fabric, it is required to reduce the electrical conductivity of the fabric as much as possible. However, in order to achieve the antistatic property of the fabric, the fabric needs to have a certain electrical conductivity to slowly release static electricity and control or reduce the accumulation of surface static electricity, thereby reducing the surface charge density. SUMMARY

[0004] In view of the deficiencies of the prior art, the present application provides a multi-layer flame-retardant composite fabric for aircraft cabin based on flame-retardant fiber and a preparation method thereof, to solve the problem that the flame-retardant performance and antistatic performance of polyamide-based fabric need to be improved in the prior art.

[0005] To achieve the above-mentioned purpose, the technical solution adopted by the present application is as follows: A preparation method of a multi-layer flame-retardant composite fabric for aircraft cabin based on flame-retardant fiber, comprising the following steps: Step one, acrylic acid is reacted with DOPO (9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide) to prepare modified DOPO; Step two, epoxy-based POSS (cage-type polyhedral oligomeric silsesquioxane) is reacted with the modified DOPO to prepare a composite flame retardant; Step three, the hydrophilic grafted polyamide (PA) is reacted with the composite flame retardant and the amino modified nano montmorillonite to prepare a modified polyamide; Step four, the modified polyamide is melt spun, cut, and a flame-retardant fiber is prepared; Step five, the flame-retardant fiber is spun into a flame-retardant yarn, and the flame-retardant yarn is spun into a fabric to obtain a surface fabric; The flame-retardant fiber is blended with the polyester fiber to obtain a blended yarn, and the blended yarn is spun into a fabric to obtain a bottom fabric; The surface fabric and the bottom fabric are compounded to obtain an aviation cabin multilayer flame-retardant composite fabric based on the flame-retardant fiber.

[0006] Preferably, the step one specifically comprises: The DOPO is mixed with the acrylic acid, reacted, and after the reaction is completed, a modified DOPO is obtained; The molar ratio of the DOPO to the acrylic acid is 1:1, and the reaction conditions are refluxing at a temperature of 155-165 DEG C for 2.5-3.5 h under a nitrogen atmosphere.

[0007] Preferably, the step two specifically comprises: The epoxy POSS, the polymerization inhibitor, the catalyst are added into the xylene, heated to a set temperature, the modified DOPO is added, reacted, and after the reaction is completed, purified to obtain a composite flame retardant; The molar ratio of the epoxy POSS to the modified DOPO is 1:(3-5), and the reaction conditions are reacting at a set temperature for 6-8 h, the set temperature is 90-110 DEG C, the addition amount of the xylene is 3-5 times of the mass of the epoxy POSS, the addition amount of the polymerization inhibitor is 0.1%-0.3% of the mass sum of the epoxy POSS, the xylene and the modified DOPO, and the addition amount of the catalyst is 0.4%-0.8% of the mass sum of the epoxy POSS, the xylene, the modified DOPO and the catalyst; The epoxy POSS comprises an octa-epoxy cyclohexyl ethyl POSS, the polymerization inhibitor comprises 2,6-di-tert-butyl-p-cresol, and the catalyst comprises N,N-dimethyl benzyl amine.

[0008] Preferably, the step three specifically comprises: The hydrophilic grafted polyamide is mixed with the composite flame retardant and the amino modified nano montmorillonite, melt reacted, extruded, cooled, cut into particles, and dried to obtain a modified polyamide; The mass ratio of the hydrophilic grafted polyamide, the composite flame retardant and the amino modified nano montmorillonite is 100:(3-5):(2-4), and the temperature of the melt reaction is 270-290 DEG C.

[0009] Preferably, the amino modified nano montmorillonite is prepared by the following steps: adding γ-aminopropyl triethoxysilane (silane coupling agent KH-550) into the aqueous ethanol solution, adjusting the pH value to 3.5-4.5 to obtain a γ-aminopropyl triethoxysilane solution; adding the γ-aminopropyl triethoxysilane solution into the nanometer montmorillonite dispersion liquid, reacting, purifying and drying after the reaction to obtain the amino-modified nanometer montmorillonite; The mass ratio of the nanometer montmorillonite dispersion liquid, the γ-aminopropyl triethoxysilane and the aqueous ethanol solution is 50:(0.5-1.5):(10-20), and the reaction condition is 3.5-4.5 h at 55-65℃.

[0010] Preferably, the aqueous ethanol solution comprises 95wt% aqueous ethanol solution; the nanometer montmorillonite dispersion liquid is prepared by nanometer montmorillonite and chloroform, and the mass percentage of nanometer montmorillonite in the nanometer montmorillonite dispersion liquid is 5%-9%.

[0011] Preferably, the hydrophilic grafted polyamide is prepared by the following steps: adding the polyamide resin powder into the aqueous potassium persulfate solution, pre-irradiating under stirring, filtering and drying after the reaction to obtain the pre-irradiated polyamide resin powder; The mass ratio of the polyamide resin powder and the aqueous potassium persulfate solution is 1:(20-30), and the reaction condition is 1-2 h at 70-80℃, and the aqueous potassium persulfate solution is 0.5wt% aqueous potassium persulfate solution; adding the pre-irradiated polyamide resin powder into the hydrophilic monomer solution, reacting, filtering, washing and drying after the reaction to obtain the hydrophilic grafted polyamide; The mass ratio of the pre-irradiated polyamide resin powder and the hydrophilic monomer solution is 1:(30-50), and the reaction condition is 1.5-2.5 h at 70-90℃, and the hydrophilic monomer solution is prepared by the 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, and the total amount of 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate in the hydrophilic monomer solution is 20wt%.

[0012] Preferably, in the step four, the process parameters of the melt spinning include: the melt temperature is 280-300℃, the number of the spinneret holes is 15-30, the hole diameter is 0.1-0.2mm, the winding speed is 300-500m / min, and the winding temperature is 18-19℃. The obtained flame-retardant fiber monofilament fineness is 0.8-3dtex.

[0013] Preferably, in the step five, the yarn count of the flame-retardant yarn is 8-50S (English count), and the gram weight of the surface fabric is 100-500g / m 2 .

[0014] Preferably, in the step five, the mass ratio of the flame-retardant fiber to the polyester fiber is 1:(1-3), the yarn count of the blended yarn is 8-50S, and the gram weight of the bottom fabric is 100-500g / m 2 .

[0015] A flame-retardant fiber-based multi-layer flame-retardant composite fabric for aircraft cabin prepared by the preparation method of the flame-retardant fiber-based multi-layer flame-retardant composite fabric for aircraft cabin.

[0016] Compared with the prior art, the beneficial effects of the present application are: The flame-retardant fiber-based multi-layer flame-retardant composite fabric for aircraft cabin comprises a surface fabric and a bottom fabric, wherein the surface fabric is made of polyamide fiber, has good wear resistance, and has small filament fineness, belongs to superfine fiber, and has a soft touch; the bottom fabric is made of blended polyamide fiber and polyester fiber, has good wrinkle resistance, and is combined with the surface fabric to obtain a composite fabric with good wrinkle resistance. The polyamide fiber in the present application is a flame-retardant fiber prepared by modifying polyamide and then melt spinning, wherein the composite flame retardant is prepared 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 physical barrier, free radical capture, and carbon layer enhancement; DOPO decomposes to generate phosphorus-containing free radicals at high temperature, which can capture H· and OH· free radicals in the combustion chain reaction, inhibit flame propagation, and at the same time, form phosphoric acid or polyphosphoric acid after decomposition, promote the carbonization of the material surface, and form a carbon layer that can insulate heat and oxygen, thereby slowing down pyrolysis and flammable gas release; the synergistic effect of POSS and DOPO is good; DOPO undergoes nucleophilic addition reaction with the carbon-carbon double bond in the acrylic acid molecule through the high-reactivity P-H bond, and then undergoes ring-opening reaction with the epoxy group in the epoxy POSS molecule through the introduced carboxyl group, thereby realizing the chemical bonding of POSS and DOPO. In the present application, nano-montmorillonite is introduced during the preparation of modified polyamide, which can improve the flame retardant performance and antistatic performance of polyamide; during the melt reaction of nano-montmorillonite, polyamide, and the composite flame retardant, the nano-montmorillonite can react with the epoxy group on the epoxy POSS molecule, thereby connecting the nano-montmorillonite to the composite flame retardant molecule through a stable chemical bond. 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

[0017] 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; 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. Figure 3 The infrared spectrum of the modified DOPO prepared in Example 1 of this invention; 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. Figure 5 Line 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

[0018] 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.

[0019] Example 1

[0020] 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: 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. 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 characteristic absorption peak of P-C at 1180 cm -1 characteristic absorption peak of P=O at 1720 cm Step two, add octa-epoxy cyclohexyl ethyl POSS, 2,6-di-tert-butyl phenol, N,N-dimethyl benzyl amine into xylene, heat to 90℃, add modified DOPO, react at 90℃ for 8h, after the reaction is completed, cool to room temperature, pour out the upper layer solution, add 3 times the mass of acetone to the lower layer reactant, remove the acetone by distillation under reduced pressure, to obtain a composite flame retardant; The molar ratio of epoxy POSS to modified DOPO is 1:3, the addition amount of xylene is 3 times the mass of epoxy POSS, the addition amount of 2,6-di-tert-butyl phenol is 0.1% of the mass sum of epoxy POSS, xylene and modified DOPO, and the addition amount of N,N-dimethyl benzyl amine is 0.4% of the mass sum of epoxy POSS, xylene and modified DOPO; Step three, mix the hydrophilic grafted PA66 with the composite flame retardant and the amino modified nano montmorillonite, the mass ratio of the hydrophilic grafted PA66 to the composite flame retardant and the amino modified nano montmorillonite is 100:3:2, melt and react, the melt and reaction temperature is 270℃, extrude, cool, cut into particles and dry to obtain the modified polyamide; The amino modified nano montmorillonite is prepared by the following steps: Add γ-aminopropyl triethoxysilane into 95wt% ethanol aqueous solution, adjust the pH value to 4 to obtain a γ-aminopropyl triethoxysilane solution; Drop the γ-aminopropyl triethoxysilane solution into the nano montmorillonite dispersion liquid, react at 60℃ for 4h, after the reaction is completed, filter, wash with ethanol for 3 times, and then place in a 50℃ vacuum drying oven to dry to constant weight to obtain the amino modified nano montmorillonite; The mass ratio of the nano montmorillonite dispersion liquid, γ-aminopropyl triethoxysilane and 95wt% ethanol aqueous solution is 50:0.5:10, the nano montmorillonite dispersion liquid is prepared by nano montmorillonite and chloroform, and the mass percentage content of nano montmorillonite in the nano montmorillonite dispersion liquid is 8%; The hydrophilic grafted PA66 is prepared by the following steps: Add PA66 powder into 0.5wt% potassium persulfate aqueous solution, the mass ratio of PA66 powder to 0.5wt% potassium persulfate aqueous solution is 1:25, pre-irradiate under the condition of 300r / min stirring, the reaction condition is 75℃ for 1.5h, after the reaction is completed, filter, place in a 50℃ vacuum drying oven to dry to constant weight to obtain the pre-irradiated PA66 powder; The pre-initiated PA66 powder is added into the hydrophilic monomer solution, the mass ratio of the pre-initiated PA66 powder and the hydrophilic monomer solution is 1:40, and the reaction is carried out at 80℃ for 2h; after the reaction is completed, the product is filtered, washed with deionized water for 3 times, and dried in a vacuum drying box at 50℃ until the weight is constant to obtain the hydrophilic grafted polyamide; The hydrophilic monomer solution is prepared by mixing 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, and the total amount of 2-acrylamide-2-methylpropanesulfonic acid and hydroxyethyl methacrylate in the hydrophilic monomer solution is 20wt%; Step four, melt spinning of the modified polyamide, the process parameters of melt spinning include: the melting temperature is 280℃, the number of holes of the spinneret is 25, the hole diameter is 0.15mm, the winding speed is 400m / min, the winding temperature is 18℃, and the product is cut to obtain the flame-retardant fiber; The single filament fineness of the flame-retardant fiber is 1.5dtex, and the length of the flame-retardant fiber is 38-51mm; Step five, spinning the flame-retardant fiber into flame-retardant yarn, the yarn count of the flame-retardant yarn is 40S, and then spinning the flame-retardant yarn into a fabric to obtain a surface fabric, and the grammage of the surface fabric is 200g / m 2 ; Spinning the flame-retardant fiber and the polyester fiber to obtain a blended yarn, the mass ratio of the flame-retardant fiber and the polyester fiber is 1:1, the yarn count of the blended yarn is 40S, and then spinning the blended yarn into a fabric to obtain a bottom fabric, and the grammage of the bottom fabric is 200g / m 2 ; The surface fabric and the bottom fabric are sewn together by using a polyester sewing thread to obtain the multi-layer flame-retardant composite fabric for aviation cabin based on the flame-retardant fiber.

[0021] Example 2 The present embodiment discloses a preparation method of a multi-layer flame-retardant composite fabric for aviation cabin based on flame-retardant fiber, which comprises the following steps: Step one, mixing DOPO and acrylic acid, the molar ratio of DOPO and acrylic acid is 1:1, refluxing reaction under nitrogen atmosphere at 165℃ for 2.5h, and then cooling to room temperature to obtain modified DOPO; Step two, adding octa-epoxy cyclohexyl ethyl POSS, 2,6-di-tert-butyl phenol and N,N-dimethyl benzylamine into xylene, heating to 110℃, adding the modified DOPO, and reacting at 110℃ for 6h, then cooling to room temperature, pouring out the upper layer solution, adding 3 times the mass of acetone to the lower layer reactant, removing the acetone by reduced pressure distillation to obtain a composite flame retardant; The molar ratio of the epoxy POSS to the modified DOPO is 1:5, the adding amount of the xylene is 5 times of the mass of the epoxy POSS, the adding amount of the 2,6-di-tert-butyl-p-cresol is 0.3% of the mass sum of the epoxy POSS, the xylene and the modified DOPO, and the adding amount of the N,N-dimethylbenzylamine is 0.8% of the mass sum of the epoxy POSS, the xylene and the modified DOPO; Step three, the hydrophilic grafted PA66 is mixed with the composite flame retardant and the amino modified nanometer montmorillonite, the mass ratio of the hydrophilic grafted PA66 to the composite flame retardant and the amino modified nanometer montmorillonite is 100:5:4, melt reaction is carried out, the temperature of the melt reaction is 290 DEG C, extrusion is carried out, cooling, pelletizing and drying are carried out, and the modified polyamide is obtained; The preparation method of the amino modified nanometer montmorillonite and the hydrophilic grafted PA66 is the same as that in Embodiment 1; Step four, the modified polyamide is melt spun, the process parameters of the melt spinning include that the melt temperature is 300 DEG C, the number of the holes of the spinneret is 25, the hole diameter is 0.15 mm, the winding speed is 400 m / min, the winding temperature is 18 DEG C, and the modified polyamide is obtained by cutting; The single filament fineness of the flame-retardant fiber is 1.5 dtex, and the length of the flame-retardant fiber is 38-51 mm; Step five, the flame-retardant fiber is spun into flame-retardant yarn, the yarn count of the flame-retardant yarn is 40S, the flame-retardant yarn is spun into a fabric, and the surface layer fabric is obtained, and the grammage of the surface layer fabric is 200 g / m 2 ; The flame-retardant fiber is blended with the polyester fiber, the mass ratio of the flame-retardant fiber to the polyester fiber is 1:3, the blended yarn is obtained, the yarn count of the blended yarn is 40S, the blended yarn is spun into a fabric, and the bottom layer fabric is obtained, and the grammage of the bottom layer fabric is 200 g / m 2 ; The surface layer fabric and the bottom layer fabric are sewn together by using the polyester sewing thread and other fabrics, and the multi-layer flame-retardant composite fabric for an aviation cabin based on the flame-retardant fiber is obtained.

[0022] Embodiment 3 The embodiment discloses a preparation method of a multi-layer flame-retardant composite fabric for an aviation cabin based on a flame-retardant fiber. Step one, DOPO is mixed with acrylic acid, the molar ratio of the DOPO to the acrylic acid is 1:1, reflux reaction is carried out under a nitrogen atmosphere at a temperature of 160 DEG C for 3 h, after the reaction is completed, cooling is carried out to room temperature, and the modified DOPO is obtained; Step two, add octa-epoxy cyclohexyl ethyl POSS, 2,6-di-tert-butyl phenol, N,N-dimethyl benzylamine into xylene, heat to 100℃, add modified DOPO, react at 100℃ for 7h, after the reaction is completed, cool to room temperature, pour out the upper layer solution, add 3 times the mass of acetone to the lower layer reactant, remove the acetone under reduced pressure, to obtain the composite flame retardant; The molar ratio of epoxy POSS to modified DOPO is 1:4, the addition amount of xylene is 4 times the mass of epoxy POSS, the addition amount of 2,6-di-tert-butyl phenol is 0.15% of the mass sum of epoxy POSS, xylene and modified DOPO, and the addition amount of N,N-dimethyl benzylamine is 0.5% of the mass sum of epoxy POSS, xylene and modified DOPO; Step three, mix the hydrophilic grafted PA66 with the composite flame retardant and the amino modified nano montmorillonite, the mass ratio of the hydrophilic grafted PA66 to the composite flame retardant and the amino modified nano montmorillonite is 100:3.5:2.5, melt and react, the melt and reaction temperature is 280℃, extrude, cool, cut into particles and dry to obtain the modified polyamide; The preparation method of the amino modified nano montmorillonite and the hydrophilic grafted PA66 is the same as that in Example 1; Step four, melt and spin the modified polyamide, the process parameters of melt and spinning include: the melt temperature is 290℃, the number of holes of the spinneret is 25, the hole diameter is 0.15mm, the winding speed is 400m / min, the winding temperature is 18℃, and the short cutting is performed to obtain the flame retardant fiber; The single filament fineness of the flame retardant fiber is 1.5dtex, and the length of the flame retardant fiber is 38-51mm; Step five, spin the flame retardant fiber into flame retardant yarn, the yarn count of the flame retardant yarn is 40S, and then spin the flame retardant yarn into a fabric to obtain a surface fabric, and the grammage of the surface fabric is 200g / m 2 ; Spun the flame retardant fiber and the polyester fiber into blended yarn, the mass ratio of the flame retardant fiber to the polyester fiber is 1:1.5 to obtain blended yarn, and the yarn count of the blended yarn is 40S, and then spin the blended yarn into a fabric to obtain a bottom fabric, and the grammage of the bottom fabric is 200g / m 2 ; Spun the flame retardant fiber and the polyester fiber into blended yarn, the mass ratio of the flame retardant fiber to the polyester fiber is 1:1.5 to obtain blended yarn, and the yarn count of the blended yarn is 40S, and then spin the blended yarn into a fabric to obtain a bottom fabric, and the grammage of the bottom fabric is 200g / m

[0023] Example 4 The present embodiment discloses a preparation method of a multi-layer flame-retardant composite fabric for aviation cabin based on flame-retardant fiber, which comprises the following steps: Step one, mix DOPO with acrylic acid, the molar ratio of DOPO to acrylic acid is 1:1, reflux reaction under nitrogen atmosphere at 160℃ for 3h, after the reaction is completed, cool to room temperature, to obtain modified DOPO; Step two, add octa-epoxy cyclohexyl ethyl POSS, 2,6-di-tert-butyl phenol, N,N-dimethyl benzylamine into xylene, heat to 100℃, add modified DOPO, react at 100℃ for 7h, after the reaction is completed, cool to room temperature, pour out the upper layer solution, add 3 times the mass of acetone to the lower layer reactant, remove the acetone by reduced pressure distillation, to obtain the composite flame retardant; Wherein, the molar ratio of epoxy POSS to modified DOPO is 1:4, the addition amount of xylene is 4 times the mass of epoxy POSS, the addition amount of 2,6-di-tert-butyl phenol is 0.2% of the mass sum of epoxy POSS, xylene and modified DOPO, and the addition amount of N,N-dimethyl benzylamine is 0.6% of the mass sum of epoxy POSS, xylene and modified DOPO; Step three, mix the hydrophilic grafted PA66 with the composite flame retardant and the amino modified nano montmorillonite, the mass ratio of the hydrophilic grafted PA66 to the composite flame retardant and the amino modified nano montmorillonite is 100:4:3, melt reaction, the melt reaction temperature is 280℃, extrude, cool, cut into particles and dry to obtain the modified polyamide; The preparation method of the amino modified nano montmorillonite and the hydrophilic grafted PA66 is the same as that in embodiment 1; Step four, melt spinning the modified polyamide, the process parameters of melt spinning include: the melt temperature is 290℃, the number of holes of the spinneret is 25, the hole diameter is 0.15mm, the winding speed is 400m / min, the winding temperature is 18℃, and the chopped, to obtain the flame retardant fiber; The single filament fineness of the flame retardant fiber is 1.5dtex, and the length of the flame retardant fiber is 38-51mm; Step five, spin the flame retardant fiber into flame retardant yarn, the yarn count of the flame retardant yarn is 40S, and then spin the flame retardant yarn into fabric to obtain the surface layer fabric, and the grammage of the surface layer fabric is 200g / m 2 ; Spun the flame retardant fiber and the polyester fiber into blended yarn, the mass ratio of the flame retardant fiber to the polyester fiber is 1:2, to obtain the blended yarn, and the yarn count of the blended yarn is 40S, and then spin the blended yarn into fabric to obtain the bottom layer fabric, and the grammage of the bottom layer fabric is 200g / m 2 ; Spun the flame retardant fiber and the polyester fiber into blended yarn, the mass ratio of the flame retardant fiber to the polyester fiber is 1:2, to obtain the blended yarn, and the yarn count of the blended yarn is 40S, and then spin the blended yarn into fabric to obtain the bottom layer fabric, and the grammage of the bottom layer fabric is 200g / m

[0024] Example 5 The embodiment discloses a preparation method of a multilayer flame-retardant composite fabric based on flame-retardant fibers for an aircraft cabin. Step one, mix DOPO with acrylic acid, the molar ratio of DOPO to acrylic acid is 1:1, reflux reaction under nitrogen atmosphere at 160 DEG C for 3h, after the reaction, cool to room temperature, get modified DOPO; Step two, add octa-epoxy cyclohexyl ethyl POSS, 2, 6-di-tert-butyl phenol, N, N-dimethyl benzyl amine into xylene, heat to 100 DEG C, add modified DOPO, react at 100 DEG C for 7h, after the reaction, cool to room temperature, pour out the upper layer solution, add 3 times the mass of acetone to the lower layer reactant, remove acetone by reduced pressure distillation, get composite flame retardant; Wherein, the molar ratio of epoxy POSS to modified DOPO is 1:4, the addition amount of xylene is 4 times the mass of epoxy POSS, the addition amount of 2, 6-di-tert-butyl phenol is 0.25% of the mass sum of epoxy POSS, xylene and modified DOPO, and the addition amount of N, N-dimethyl benzyl amine is 0.7% of the mass sum of epoxy POSS, xylene and modified DOPO; Step three, mix hydrophilic grafting PA66 with composite flame retardant and amino modified nano montmorillonite, the mass ratio of hydrophilic grafting PA66 to composite flame retardant and amino modified nano montmorillonite is 100:4.5:3.5, melt reaction, the melt reaction temperature is 280 DEG C, extrude, cool, cut into particles and dry to get modified polyamide; The preparation method of the amino modified nano montmorillonite and the hydrophilic grafting PA66 is the same as that in embodiment 1; Step four, melt spinning of the modified polyamide, the process parameters of melt spinning include: the melt temperature is 290 DEG C, the number of holes of the spinneret is 25, the hole diameter is 0.15mm, the winding speed is 400m / min, the winding temperature is 18 DEG C, and the short cutting is carried out to prepare flame-retardant fibers; The fineness of the flame-retardant fiber single filament is 1.5dtex, and the length of the flame-retardant fiber is 38-51mm; Step five, spin the flame-retardant fibers into flame-retardant yarns, the yarn count of the flame-retardant yarns is 40S, then spin the flame-retardant yarns into a fabric to get a surface layer fabric, and the grammage of the surface layer fabric is 200g / m 2 ; Mix the flame-retardant fibers with polyester fibers, the mass ratio of the flame-retardant fibers to the polyester fibers is 1:2.5 to get a blended yarn, the yarn count of the blended yarn is 40S, then spin the blended yarn into a fabric to get a bottom layer fabric, and the grammage of the bottom layer fabric is 200g / m 2 ; The surface layer fabric and the bottom layer fabric are sewn together by using polyester sewing thread and other fabrics to get a multilayer flame-retardant composite fabric based on flame-retardant fibers for an aircraft cabin.

[0025] Comparative Example 1 The present comparative example discloses a preparation method of a multilayer flame-retardant composite fabric for aircraft cabin based on flame-retardant fibers, comprising the following steps: Step one, mix DOPO with acrylic acid, the molar ratio of DOPO to acrylic acid is 1:1, reflux reaction under nitrogen atmosphere at 155℃ for 3.5h, after the reaction is completed, cool to room temperature to obtain modified DOPO; Step two, add octa-epoxy cyclohexyl ethyl POSS, 2,6-di-tert-butyl-p-cresol, N,N-dimethyl benzylamine into xylene, heat to 90℃, add modified DOPO, react at 90℃ for 8h, after the reaction is completed, cool to room temperature, pour out the upper layer solution, add 3 times the mass of acetone to the lower layer reactant, remove acetone by reduced pressure distillation to obtain a composite flame retardant; Wherein, the molar ratio of epoxy POSS to modified DOPO is 1:3, the addition amount of xylene is 3 times the mass of epoxy POSS, the addition amount of 2,6-di-tert-butyl-p-cresol is 0.1% of the mass sum of epoxy POSS, xylene and modified DOPO, and the addition amount of N,N-dimethyl benzylamine is 0.4% of the mass sum of epoxy POSS, xylene and modified DOPO; Step three, mix PA66 powder with the composite flame retardant and amino modified nano montmorillonite, the mass ratio of PA66 powder to the composite flame retardant and amino modified nano montmorillonite is 100:3:2, melt and react, the melt and reaction temperature is 270℃, extrude, cool, cut and dry to obtain modified polyamide; The preparation method of the amino modified nano montmorillonite is the same as that of Example 1; Step four, melt and spin the modified polyamide, the process parameters of melt and spinning include: melt temperature is 280℃, the number of holes of the spinneret is 25, the hole diameter is 0.15mm, the winding speed is 400m / min, the winding temperature is 18℃, and the chopped, to obtain flame-retardant fibers; The single filament fineness of the flame-retardant fibers is 1.5dtex, and the length of the flame-retardant fibers is 38-51mm; Step five, spin the flame-retardant fibers into flame-retardant yarns, the yarn count of the flame-retardant yarns is 40S, then spin the flame-retardant yarns into a fabric to obtain a surface layer fabric, and the grammage of the surface layer fabric is 200g / m 2 ; Mix the flame-retardant fibers with polyester fibers, the mass ratio of the flame-retardant fibers to the polyester fibers is 1:1 to obtain a blended yarn, the yarn count of the blended yarn is 40S, then spin the blended yarn into a fabric to obtain a bottom layer fabric, and the grammage of the bottom layer fabric is 200g / m 2 ; The surface fabric and the bottom fabric are sewn and compounded by a polyester sewing thread and the like, to obtain the multi-layer flame-retardant composite fabric for aviation cabin based on the flame-retardant fiber.

[0026] Comparative Example 2 The present comparative example discloses a preparation method of a multi-layer flame-retardant composite fabric for aviation cabin based on flame-retardant fiber, comprising the following steps: Step one, PA66 powder is mixed with DOPO, octa-epoxy cyclohexyl ethyl POSS and nano-montmorillonite, and the mass ratio of PA66 powder, DOPO, octa-epoxy cyclohexyl ethyl POSS and nano-montmorillonite is 100.4:1.9:0.9:1.8, melt reaction, extrusion, cooling, granulation, drying, to obtain modified polyamide; Step two, melt spinning the modified polyamide, and the process parameters of melt spinning include: melt temperature is 280℃, the number of holes of the spinneret is 25, the hole diameter is 0.15mm, the winding speed is 400m / min, the winding temperature is 18℃, and the chopped, to obtain the flame-retardant fiber; The flame-retardant fiber single filament fineness is 1.5dtex, and the length of the flame-retardant fiber is 38-51mm; Step three, spinning the flame-retardant fiber into flame-retardant yarn, and the yarn count of the flame-retardant yarn is 40S, and then spinning the flame-retardant yarn into fabric to obtain the surface fabric, and the grammage of the surface fabric is 200g / m 2 ; Spinning the flame-retardant fiber and the polyester fiber, and the mass ratio of the flame-retardant fiber and the polyester fiber is 1:1, to obtain the blended yarn, and the yarn count of the blended yarn is 40S, and then spinning the blended yarn into fabric to obtain the bottom fabric, and the grammage of the bottom fabric is 200g / m 2 ; The surface fabric and the bottom fabric are sewn and compounded by a polyester sewing thread and the like, to obtain the multi-layer flame-retardant composite fabric for aviation cabin based on the flame-retardant fiber.

[0027] In the above examples and comparative examples, the nano-montmorillonite is purchased from Guangzhou Yifeng Chemical Co., Ltd., model: TY-710C, particle size: 50nm; the PA66 powder is purchased from Dongguan Weicai Plastic Raw Material Co., Ltd., specification: 200 mesh, melt temperature: 255℃; the polyester fiber is purchased from Shandong Oude Chemical Fiber Products Co., Ltd., single filament fineness is 0.5D, length is 4mm; the polyester sewing thread is purchased from Yiwu Shenkai Thread Co., Ltd., specification: 40S / 2.

[0028] Test Example (1) Flame retardant performance: the surface layer fabric prepared from Example 1-5 and Comparative Example 1-2 is cut into a sample of 150mm x 58mm, and the limiting oxygen index value of the sample is measured: the sample is placed in a glass tank supported by a rectangular frame, when the surrounding reaches a stable oxygen concentration, the sample is ignited from the upper end, the flame height of the igniter is about 20mm, when the combustion time of the fabric is less than 30s, the oxygen concentration is the critical oxygen concentration required for the combustion of the fabric, that is, the limiting oxygen index value; the surface layer fabric prepared from Example 1-5 and Comparative Example 1-2 is cut into a sample of 300mm x 80mm, and the damage length of the sample is measured: the sample is clamped with a rectangular sample clamp and vertically hung in a reaction box, a layer of absorbent cotton is placed below, the ignition time is selected to be 12s, the flame height is controlled to be 40mm, and the damage length during combustion is recorded, and the measurement results are shown in Table 1: Table 1

[0029] As shown in Table 1, the surface layer fabric prepared by the application has good flame retardant performance, which can further improve the flame retardant performance of the composite fabric. POSS and DOPO are used as flame retardant components, and the two components have a synergistic effect, and the flame retardant effect is good. In addition, the connection between POSS and DOPO is through a stable chemical bond, and then the connection is introduced into the polyamide molecule. The compatibility and uniformity between the composite flame retardant and the polyamide are good, and the flame retardant performance of the polyamide is good. In addition, the introduction of nano-montmorillonite further improves the flame retardant performance. Compared with Example 1, in Comparative Example 1, the polyamide is not modified by hydrophilic grafting, that is, no hydrophilic groups are introduced, and the composite flame retardant can only be bonded with the amine group and the carboxyl group at the end of the polyamide molecule. The compatibility and uniformity between the composite flame retardant and the nano-montmorillonite and the polyamide are decreased, and the flame retardant performance is decreased. Compared with Comparative Example 1, in Comparative Example 2, there is no bonding between POSS, DOPO and nano-montmorillonite, that is, only POSS can be bonded with the amine group and the carboxyl group at the end of the polyamide molecule through the epoxy group, and the flame retardant performance is further decreased.

[0030] (2) Antistatic property: the charge surface density of the surface layer fabric prepared from Example 1-5 and Comparative Example 1-2 is measured according to the standard GB / T12703.2-2009 "Evaluation of static property of textiles Part 2: Charge surface density", and the measurement results are shown in Table 2: Table 2

[0031] It can be seen from Table 2 that the surface fabric prepared by the application has good antistatic property. The polyamide is modified by hydrophilic grafting, and hydrophilic groups such as hydroxyl and carboxyl are introduced, so that the antistatic property of the polyamide is improved, and the nano-montmorillonite is introduced, so that the antistatic property of the polyamide is improved. Compared with Example 1, in Comparative Example 1, the polyamide is not modified by hydrophilic grafting, and the bonding amount of the nano-montmorillonite and the polyamide is reduced, so that the antistatic property is obviously reduced; compared with Comparative Example 1, in Comparative Example 2, the compatibility and dispersion uniformity between the nano-montmorillonite and the polyamide are further reduced, and the antistatic property is further reduced.

[0032] Although embodiments of the application have been shown and described, it is to be understood that various modifications, substitutions, alternatives and variations can be made to these embodiments without departing from the principles and spirit of the application, 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; Step 2: React epoxy group POSS with modified DOPO to prepare a composite flame retardant; Step 3: React hydrophilic grafted polyamide with composite flame retardant and amino-modified nano-montmorillonite to prepare modified polyamide; 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 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.

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 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. 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, Step three specifically includes: 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; 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℃.

5. The method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers according to claim 4, 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℃.

6. The method for preparing a multi-layer flame-retardant composite fabric for aircraft cabins based on flame-retardant fibers according to claim 4, characterized in that, 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%.

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 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.

8. 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 .

9. 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 surface fabric is 100-500g / m². 2 .

10. 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 1-9.

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