Lightweight thermal layered composite fabric, method of making and application on an aircraft cabin quilt

Abstract

The application relates to the technical field of layered fabrics, and discloses a light-weight warm-keeping layered composite fabric, a preparation method and application in an aviation cabin cotton quilt. An organic-inorganic composite flame retardant is prepared by grafting and compounding a flame retardant and far-infrared material graphene oxide, and the flame retardant is used for surface finishing of polyester-cotton fabric, so that the fabric is endowed with persistent flame-retardant performance and far-infrared heating performance; the fabric is used as a surface layer and an inner layer fabric; a multi-layer composite structure of the surface layer and the inner layer fabric heating flame-retardant, the middle layer regenerated polyester flake light-weight warm-keeping is constructed; the warm-keeping and flame-retardant performance of the layered composite fabric are improved; and the layered composite fabric is better applied in the aviation cabin cotton quilt.

Description

Technical Field

[0001] This invention relates to the field of layered fabric technology, specifically to a lightweight, warm, layered composite fabric, its preparation method, and its application in aircraft cabin quilts. Background Technology

[0002] Layered composite fabrics are multi-layered structural materials formed by combining fabrics of different properties through physical or chemical methods, and are widely used in the textile industry. Through proper design and combination, they can achieve multiple functions that are difficult to achieve with a single fabric, such as warmth and flame retardancy. In applications such as aviation where safety and comfort are paramount, the technological value of layered composite fabrics is particularly prominent.

[0003] To improve the warmth retention of fabrics, most existing technologies involve increasing the number of layers in the composite fabric and the thickness of the filling layer. However, this often leads to an increase in the overall weight of the fabric, which contradicts the lightweight requirements of fields such as aerospace. In recent years, the introduction of far-infrared heat storage technology has provided a new approach to lightweight warmth retention. However, how to rationally utilize far-infrared functional materials in fabrics and synergistically enhance their effects with other layer materials remains a technical problem that is currently being explored.

[0004] From a flame-retardant perspective, textiles used in aircraft cabins must meet fire safety standards. Current technologies typically employ flame-retardant fibers or agents to improve the flame-retardant properties of fabrics. However, the bonding strength between flame retardants and fabrics is limited, and washability is insufficient, making it difficult to maintain a stable flame-retardant rating during long-term use and maintenance.

[0005] In conclusion, developing a layered composite fabric that combines lightweight warmth and durable flame retardancy is of great significance for meeting the needs of applications such as aircraft cabin quilts. Summary of the Invention

[0006] The purpose of this invention is to overcome the shortcomings of the prior art and provide a lightweight, warm, layered composite fabric, its preparation method, and its application in aircraft cabin quilts. An organic-inorganic composite flame retardant is prepared by grafting a flame retardant with far-infrared material graphene oxide. This flame retardant is then used to surface-finish a polyester-cotton fabric, endowing it with durable flame-retardant properties and far-infrared heating properties. This fabric is then used as both the outer and inner layers. By constructing a multi-layered composite structure with a heat-generating and flame-retardant outer and inner layers and a lightweight, warm, recycled polyester wadding middle layer, the warmth and flame-retardant properties of the layered composite fabric are improved, thus enabling its better application in aircraft cabin quilts.

[0007] To achieve the above objectives, the technical solution adopted by the present invention is as follows: A method for preparing a thermal insulating layered composite fabric includes the following steps: Step (1): Add 1,4-dioxane and triethylamine to hydroquinone in sequence, stir to dissolve, add hexachlorocyclotriphosphazene solution dropwise, react, and after the reaction is completed, purify to obtain phenolized cyclotriphosphazene; Phenolicized cyclotriphosphazene and epichlorohydrin were mixed and reacted. After the reaction was completed, the temperature was lowered, and an aqueous sodium hydroxide solution was added to continue the reaction. After the reaction was completed, the mixture was purified to obtain epoxidized cyclotriphosphazene. Step (2): Mix graphene oxide with N,N-dimethylformamide, disperse by ultrasonication, add N,N-dimethylformamide solution of maleic anhydride, react, centrifuge, wash, and dry to obtain maleic anhydride-grafted graphene oxide. Maleic anhydride-grafted graphene oxide was mixed with N,N-dimethylformamide, ultrasonically dispersed, and then DOPO was added. After the reaction was completed, the mixture was filtered, washed, and dried to obtain DOPO-grafted graphene oxide. DOPO-grafted graphene oxide was mixed with N,N-dimethylformamide, ultrasonically dispersed, and then epoxidized triphosphazene was added. After the reaction was completed, the mixture was filtered, washed, and dried to obtain the flame retardant. Step (3): Wash and dry the polyester-cotton fabric to obtain the pre-treated polyester-cotton fabric. Flame retardant is ultrasonically dispersed in water to prepare finishing solution. Pretreated polyester-cotton fabric is immersed in finishing solution and baked to obtain surface fabric and inner fabric respectively. Step (4): Mix the recycled polyester fiber, hollow polyester fiber and ES fiber evenly, form a fiber web by dry web forming, and then reinforce it by thermal bonding to obtain recycled polyester wadding. Recycled polyester wadding is used as the middle layer fabric. The layers are stacked and aligned in the order of the outer layer fabric, the middle layer fabric, and the inner layer fabric, and then sewn together to obtain a warm, layered composite fabric.

[0008] Preferably, in step (1), when preparing phenolated triphosphazene: the ratio of hydroquinone, hexachlorocyclotriphosphazene, 1,4-dioxane, and triethylamine is 33-34:17-18:100-120mL:30-32g; the hexachlorocyclotriphosphazene solution is prepared by mixing hexachlorocyclotriphosphazene and 1,4-dioxane at a ratio of 17-18g:100mL; the dropping conditions of the hexachlorocyclotriphosphazene solution are: heating to 70-80℃ in a nitrogen atmosphere and dropping at a rate of 1-2 seconds / drop; the reaction conditions are: reacting at 70-80℃ in a nitrogen atmosphere for 12-14 hours.

[0009] Preferably, in step (1), when preparing phenolic triphosphazene, the purification conditions are as follows: filter to remove triethylamine hydrochloride, concentrate by rotary evaporation, extract with ethyl acetate, take the organic phase, add anhydrous sodium sulfate to dry, concentrate by rotary evaporation again and then dry.

[0010] Preferably, in step (1), when preparing epoxidized cyclotriphosphazene, the ratio of phenolized cyclotriphosphazene, epichlorohydrin, and 30wt% sodium hydroxide aqueous solution is 20-30g: 180-220g: 10-12g; the reaction conditions are: reacting at 100-115℃ for 1h; and the conditions for continued reaction are: continuing the reaction at 50-60℃ for 2-3h.

[0011] Preferably, in step (1), when preparing epoxidized triphosphazene, the purification conditions are as follows: cooling to room temperature, vacuum filtration, taking the filtrate, rotary evaporation concentration, extraction with dichloromethane, taking the organic phase, adding anhydrous sodium sulfate for drying, rotary evaporation concentration again, and drying at room temperature.

[0012] Preferably, in step (2), when preparing maleic anhydride-grafted graphene oxide: the N,N-dimethylformamide solution of maleic anhydride is prepared by mixing 2g of maleic anhydride with 20mL of N,N-dimethylformamide; the ratio of graphene oxide, N,N-dimethylformamide, and the N,N-dimethylformamide solution of maleic anhydride is 0.5g:100-120mL:15-30mL; the reaction conditions are: reaction at 70-90℃ for 20-30h in a nitrogen atmosphere.

[0013] Preferably, in step (2), when preparing DOPO-grafted graphene oxide, the ratio of maleic anhydride-grafted graphene oxide, N,N-dimethylformamide, and DOPO is 0.5g:100-150mL:4.3-4.5g, and the reaction conditions are: reaction at 120-130℃ for 24-28h in a nitrogen atmosphere.

[0014] Preferably, in step (2), when preparing the flame retardant, the ratio of DOPO-grafted graphene oxide, N,N-dimethylformamide, and epoxidized triphosphazene is 0.5g:100-140mL:10-15g; the reaction conditions are: reaction in a nitrogen atmosphere at 130-160℃ for 18-32h.

[0015] Preferably, in step (3): the amount of flame retardant in the finishing liquid is 50-100g / L; the impregnation conditions are: a bath ratio of 1:30-50, impregnation at room temperature for 30-50min, two dips and two rolls, and a roll residue of 70-80%; the baking conditions are: pre-baking at 70-90℃ for 3-5min, and baking at 130-180℃ for 1-3min.

[0016] Preferably, in step (4): the mass ratio of recycled polyester fiber, hollow polyester fiber, and ES fiber is 62-70:16-20:14-18; the fiber arrangement direction in the fiber web is cross-arranged; the dry web forming conditions are: conveying speed of 13-15 m / s and web forming speed of 35-40 m / s; the thermal bonding reinforcement conditions are: reinforcement temperature of 150-180℃ and output temperature of 12-15 m / s; the basis weight of the recycled polyester wadding is 100-130 g / m². 2 .

[0017] Preferably, a lightweight thermal layered composite fabric is prepared using the preparation method of the thermal layered composite fabric described above.

[0018] Preferably, the application of a lightweight, thermally insulating layered composite fabric as described above in aircraft cabin quilts.

[0019] Compared with the prior art, the beneficial effects of the present invention are as follows: This invention prepares an organic-inorganic composite flame retardant by grafting a flame retardant with far-infrared material graphene oxide. This flame retardant is then used to surface-finish polyester-cotton fabric, endowing the fabric with durable flame retardant and far-infrared heating properties. This fabric is then used as the top and bottom layers. By constructing a multi-layered composite structure with heat-generating and flame-retardant top and bottom layers and lightweight and warm recycled polyester wadding in the middle layer, the warmth and flame retardant properties of the layered composite fabric are improved, making it better suited for use in aircraft cabin quilts.

[0020] This invention involves reacting hydroquinone with hexachlorocyclotriphosphazene to generate phenolic hydroxyl-terminated cyclotriphosphazene, then reacting epichlorohydrin with the phenolic hydroxyl groups to generate epoxy cyclotriphosphazene with epoxy groups at the end. Finally, the carboxyl groups on the surface of DOPO-grafted graphene oxide react with the epoxy groups to prepare an organic-inorganic composite flame retardant linked by covalent bonds. By controlling the feed ratio to ensure an excess of epoxy cyclotriphosphazene, some unreacted epoxy groups are retained in the prepared flame retardant. During the subsequent padding process, the epoxy groups chemically bond with active groups such as hydroxyl groups on the surface of the polyester / cotton fabric fibers, thereby fixing the flame retardant on the fabric surface and endowing the fabric with durable, washable flame retardant properties and far-infrared heating properties.

[0021] In this invention, low-weight recycled polyester wadding is prepared by dry web formation and thermal bonding technology after mixing recycled polyester fibers, hollow polyester fibers and ES fibers. As the middle layer of the composite fabric, it has excellent heat insulation effect and enhances the overall warmth performance of the composite fabric while achieving the goal of lightweight fabric. Attached Figure Description

[0022] Figure 1This is a bar chart showing the temperature difference of the thermal insulation layered composite fabrics prepared in Examples 1-5 and Comparative Examples 1-2 during performance testing. Figure 2 This is a bar chart showing the limiting oxygen index of the thermal insulation layered composite fabrics prepared in Examples 1-5 and Comparative Examples 1-2 of this invention during performance testing. Figure 3 This is a schematic diagram of the reaction for preparing epoxidized cyclotriphosphazene in this invention. Detailed Implementation

[0023] The present invention will be further illustrated below through specific embodiments. The following embodiments are specific implementations of the present invention, but the implementation of the present invention is not limited to the following embodiments. Any changes, modifications, substitutions, combinations, or simplifications made without departing from the spirit and principle of the present invention shall be considered equivalent substitutions and are included within the protection scope of the present invention.

[0024] Example 1 This embodiment discloses a method for preparing a thermal insulating layered composite fabric, including the following steps: Step (1): Dissolve 17.38 g of hexachlorocyclotriphosphazene in 100 mL of 1,4-dioxane to obtain a hexachlorocyclotriphosphazene solution; add 100 mL of 1,4-dioxane and 30.36 g of triethylamine to 33.04 g of hydroquinone, stir and dissolve in a nitrogen atmosphere, heat to 80 °C, add the hexachlorocyclotriphosphazene solution dropwise at a rate of 2 seconds / drop, after the addition is complete, react at 80 °C for 12 h, after the reaction is complete, filter to remove triethylamine hydrochloride, concentrate by rotary evaporation, extract with ethyl acetate, take the organic phase, dry with anhydrous sodium sulfate, concentrate again by rotary evaporation, and dry at 50 °C for 12 h to obtain phenolized cyclotriphosphazene; 30g of phenolized cyclotriphosphazene and 200g of epichlorohydrin were mixed and reacted at 110℃ for 1h. After the reaction was completed, the temperature was lowered to 60℃ and 12g of 30wt% sodium hydroxide aqueous solution was added. The reaction was carried out at 60℃ for 2h. After the reaction was completed, the mixture was cooled to room temperature, filtered under reduced pressure, and the filtrate was collected. The mixture was concentrated by rotary evaporation and extracted with dichloromethane. The organic phase was collected, dried with anhydrous sodium sulfate, concentrated again by rotary evaporation, and dried at room temperature for 12h to obtain epoxidized cyclotriphosphazene. Step (2): Mix 0.5g of graphene oxide with 120mL of N,N-dimethylformamide, sonicate for 30min, add 20mL of N,N-dimethylformamide solution of maleic anhydride, react in a nitrogen atmosphere at 80℃ for 24h, after the reaction is completed, centrifuge to collect the precipitate, wash with ethanol, and dry at 50℃ for 12h to obtain maleic anhydride-grafted graphene oxide; The N,N-dimethylformamide solution of maleic anhydride was prepared by mixing 2g of maleic anhydride with 20mL of N,N-dimethylformamide. 0.5 g of maleic anhydride-grafted graphene oxide was mixed with 140 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 4.32 g of DOPO was added, and the mixture was reacted at 130 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered, washed with ethanol, and dried at 50 °C for 12 h to obtain DOPO-grafted graphene oxide. 0.5 g of DOPO-grafted graphene oxide was mixed with 120 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 11.3 g of epoxidized triphosphazene was added, and the mixture was reacted at 150 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered and washed successively with N,N-dimethylformamide, ethanol, and water. The precipitate was then dried at 50 °C for 24 h to obtain the flame retardant. Step (3): Wash the polyester-cotton fabric with ethanol and water at room temperature, and dry it at 80°C for 5 minutes to obtain the pretreated polyester-cotton fabric. Flame retardant was ultrasonically dispersed in water to prepare a finishing solution with a flame retardant dosage of 50 g / L. The pretreated polyester-cotton fabric was immersed in the finishing solution at room temperature with a liquor ratio of 1:30 and an immersion time of 30 min. The fabric was then dipped and rubbed twice with a pick-up rate of 70%. It was then pre-dried at 80°C for 5 min and baked at 150°C for 2 min to obtain the surface fabric and the inner fabric, respectively. Step (4): Mix the recycled polyester fiber, hollow polyester fiber, and ES fiber evenly, form a web using a dry web-forming method, and then reinforce it using a thermal bonding method to obtain a web with a basis weight of 100 g / m². 2 Recycled polyester flakes; The mass ratio of recycled polyester fiber, hollow polyester fiber, and ES fiber is 70:16:14; the fiber arrangement direction in the fiber web is cross-arranged; the dry web forming conditions are: conveying speed of 13m / s and web forming speed of 40m / s; the thermal bonding reinforcement method conditions are: reinforcement temperature of 180℃ and output temperature of 12m / s. Recycled polyester wadding is used as the middle layer fabric. The layers are aligned in the order of the outer layer fabric, the middle layer fabric, and the inner layer fabric, and then sewn together using a multi-layer fabric quilting machine to obtain a warm, layered composite fabric.

[0025] Example 2 This embodiment discloses a method for preparing a thermal insulating layered composite fabric, including the following steps: Step (1): Dissolve 17.38 g of hexachlorocyclotriphosphazene in 100 mL of 1,4-dioxane to obtain a hexachlorocyclotriphosphazene solution; add 100 mL of 1,4-dioxane and 30.36 g of triethylamine to 33.04 g of hydroquinone, stir and dissolve in a nitrogen atmosphere, heat to 80 °C, add the hexachlorocyclotriphosphazene solution dropwise at a rate of 2 seconds / drop, after the addition is complete, react at 80 °C for 12 h, after the reaction is complete, filter to remove triethylamine hydrochloride, concentrate by rotary evaporation, extract with ethyl acetate, take the organic phase, dry with anhydrous sodium sulfate, concentrate again by rotary evaporation, and dry at 50 °C for 12 h to obtain phenolized cyclotriphosphazene; 30g of phenolized cyclotriphosphazene and 200g of epichlorohydrin were mixed and reacted at 110℃ for 1h. After the reaction was completed, the temperature was lowered to 60℃ and 12g of 30wt% sodium hydroxide aqueous solution was added. The reaction was carried out at 60℃ for 2h. After the reaction was completed, the mixture was cooled to room temperature, filtered under reduced pressure, and the filtrate was collected. The mixture was concentrated by rotary evaporation and extracted with dichloromethane. The organic phase was collected, dried with anhydrous sodium sulfate, concentrated again by rotary evaporation, and dried at room temperature for 12h to obtain epoxidized cyclotriphosphazene. Step (2): Mix 0.5g of graphene oxide with 120mL of N,N-dimethylformamide, sonicate for 30min, add 20mL of N,N-dimethylformamide solution of maleic anhydride, react in a nitrogen atmosphere at 80℃ for 24h, after the reaction is completed, centrifuge to collect the precipitate, wash with ethanol, and dry at 50℃ for 12h to obtain maleic anhydride-grafted graphene oxide; The N,N-dimethylformamide solution of maleic anhydride was prepared by mixing 2g of maleic anhydride with 20mL of N,N-dimethylformamide. 0.5 g of maleic anhydride-grafted graphene oxide was mixed with 140 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 4.32 g of DOPO was added, and the mixture was reacted at 130 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered, washed with ethanol, and dried at 50 °C for 12 h to obtain DOPO-grafted graphene oxide. 0.5 g of DOPO-grafted graphene oxide was mixed with 120 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 11.3 g of epoxidized triphosphazene was added, and the mixture was reacted at 150 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered and washed successively with N,N-dimethylformamide, ethanol, and water. The precipitate was then dried at 50 °C for 24 h to obtain the flame retardant. Step (3): Wash the polyester-cotton fabric with ethanol and water at room temperature, and dry it at 80°C for 5 minutes to obtain the pretreated polyester-cotton fabric. Flame retardant was ultrasonically dispersed in water to prepare a finishing solution with a flame retardant dosage of 65 g / L. The pretreated polyester-cotton fabric was immersed in the finishing solution at room temperature with a liquor ratio of 1:30 and an immersion time of 30 min. The fabric was then dipped and rubbed twice with a pick-up rate of 70%. It was then pre-dried at 80°C for 5 min and baked at 150°C for 2 min to obtain the surface fabric and the inner fabric, respectively. Step (4): Mix the recycled polyester fiber, hollow polyester fiber, and ES fiber evenly, form a web using a dry web-forming method, and then reinforce it using a thermal bonding method to obtain a web with a basis weight of 100 g / m². 2 Recycled polyester flakes; The mass ratio of recycled polyester fiber, hollow polyester fiber, and ES fiber is 68:17:15; the fiber arrangement direction in the fiber web is cross-arranged; the dry web forming conditions are: conveying speed of 13m / s and web forming speed of 40m / s; the thermal bonding reinforcement method conditions are: reinforcement temperature of 180℃ and output temperature of 12m / s. Recycled polyester wadding is used as the middle layer fabric. The layers are aligned in the order of the outer layer fabric, the middle layer fabric, and the inner layer fabric, and then sewn together using a multi-layer fabric quilting machine to obtain a warm, layered composite fabric.

[0026] Example 3 This embodiment discloses a method for preparing a thermal insulating layered composite fabric, including the following steps: Step (1): Dissolve 17.38 g of hexachlorocyclotriphosphazene in 100 mL of 1,4-dioxane to obtain a hexachlorocyclotriphosphazene solution; add 100 mL of 1,4-dioxane and 30.36 g of triethylamine to 33.04 g of hydroquinone, stir and dissolve in a nitrogen atmosphere, heat to 80 °C, add the hexachlorocyclotriphosphazene solution dropwise at a rate of 2 seconds / drop, after the addition is complete, react at 80 °C for 12 h, after the reaction is complete, filter to remove triethylamine hydrochloride, concentrate by rotary evaporation, extract with ethyl acetate, take the organic phase, dry with anhydrous sodium sulfate, concentrate again by rotary evaporation, and dry at 50 °C for 12 h to obtain phenolized cyclotriphosphazene; 30g of phenolized cyclotriphosphazene and 200g of epichlorohydrin were mixed and reacted at 110℃ for 1h. After the reaction was completed, the temperature was lowered to 60℃ and 12g of 30wt% sodium hydroxide aqueous solution was added. The reaction was carried out at 60℃ for 2h. After the reaction was completed, the mixture was cooled to room temperature, filtered under reduced pressure, and the filtrate was collected. The mixture was concentrated by rotary evaporation and extracted with dichloromethane. The organic phase was collected, dried with anhydrous sodium sulfate, concentrated again by rotary evaporation, and dried at room temperature for 12h to obtain epoxidized cyclotriphosphazene. Step (2): Mix 0.5g of graphene oxide with 120mL of N,N-dimethylformamide, sonicate for 30min, add 20mL of N,N-dimethylformamide solution of maleic anhydride, react in a nitrogen atmosphere at 80℃ for 24h, after the reaction is completed, centrifuge to collect the precipitate, wash with ethanol, and dry at 50℃ for 12h to obtain maleic anhydride-grafted graphene oxide; The N,N-dimethylformamide solution of maleic anhydride was prepared by mixing 2g of maleic anhydride with 20mL of N,N-dimethylformamide. 0.5 g of maleic anhydride-grafted graphene oxide was mixed with 140 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 4.32 g of DOPO was added, and the mixture was reacted at 130 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered, washed with ethanol, and dried at 50 °C for 12 h to obtain DOPO-grafted graphene oxide. 0.5 g of DOPO-grafted graphene oxide was mixed with 120 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 11.3 g of epoxidized triphosphazene was added, and the mixture was reacted at 150 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered and washed successively with N,N-dimethylformamide, ethanol, and water. The precipitate was then dried at 50 °C for 24 h to obtain the flame retardant. Step (3): Wash the polyester-cotton fabric with ethanol and water at room temperature, and dry it at 80°C for 5 minutes to obtain the pretreated polyester-cotton fabric. Flame retardant was ultrasonically dispersed in water to prepare a finishing solution with a flame retardant dosage of 75 g / L. The pretreated polyester-cotton fabric was immersed in the finishing solution at room temperature with a liquor ratio of 1:30 and an immersion time of 30 min. The fabric was then dipped and rubbed twice with a pick-up rate of 70%. It was then pre-dried at 80°C for 5 min and baked at 150°C for 2 min to obtain the surface fabric and the inner fabric, respectively. Step (4): Mix the recycled polyester fiber, hollow polyester fiber, and ES fiber evenly, form a web using a dry web-forming method, and then reinforce it using a thermal bonding method to obtain a web with a basis weight of 100 g / m². 2 Recycled polyester flakes; The mass ratio of recycled polyester fiber, hollow polyester fiber, and ES fiber is 66:18:16; the fiber arrangement direction in the web is cross-arranged; the dry web forming conditions are: conveying speed of 13m / s and web forming speed of 40m / s; the thermal bonding reinforcement conditions are: reinforcement temperature of 180℃ and output temperature of 12m / s. Recycled polyester wadding is used as the middle layer fabric. The layers are aligned in the order of the outer layer fabric, the middle layer fabric, and the inner layer fabric, and then sewn together using a multi-layer fabric quilting machine to obtain a warm, layered composite fabric.

[0027] Example 4 This embodiment discloses a method for preparing a thermal insulating layered composite fabric, including the following steps: Step (1): Dissolve 17.38 g of hexachlorocyclotriphosphazene in 100 mL of 1,4-dioxane to obtain a hexachlorocyclotriphosphazene solution; add 100 mL of 1,4-dioxane and 30.36 g of triethylamine to 33.04 g of hydroquinone, stir and dissolve in a nitrogen atmosphere, heat to 80 °C, add the hexachlorocyclotriphosphazene solution dropwise at a rate of 2 seconds / drop, after the addition is complete, react at 80 °C for 12 h, after the reaction is complete, filter to remove triethylamine hydrochloride, concentrate by rotary evaporation, extract with ethyl acetate, take the organic phase, dry with anhydrous sodium sulfate, concentrate again by rotary evaporation, and dry at 50 °C for 12 h to obtain phenolized cyclotriphosphazene; 30g of phenolized cyclotriphosphazene and 200g of epichlorohydrin were mixed and reacted at 110℃ for 1h. After the reaction was completed, the temperature was lowered to 60℃ and 12g of 30wt% sodium hydroxide aqueous solution was added. The reaction was carried out at 60℃ for 2h. After the reaction was completed, the mixture was cooled to room temperature, filtered under reduced pressure, and the filtrate was collected. The mixture was concentrated by rotary evaporation and extracted with dichloromethane. The organic phase was collected, dried with anhydrous sodium sulfate, concentrated again by rotary evaporation, and dried at room temperature for 12h to obtain epoxidized cyclotriphosphazene. Step (2): Mix 0.5g of graphene oxide with 120mL of N,N-dimethylformamide, sonicate for 30min, add 20mL of N,N-dimethylformamide solution of maleic anhydride, react in a nitrogen atmosphere at 80℃ for 24h, after the reaction is completed, centrifuge to collect the precipitate, wash with ethanol, and dry at 50℃ for 12h to obtain maleic anhydride-grafted graphene oxide; The N,N-dimethylformamide solution of maleic anhydride was prepared by mixing 2g of maleic anhydride with 20mL of N,N-dimethylformamide. 0.5 g of maleic anhydride-grafted graphene oxide was mixed with 140 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 4.32 g of DOPO was added, and the mixture was reacted at 130 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered, washed with ethanol, and dried at 50 °C for 12 h to obtain DOPO-grafted graphene oxide. 0.5 g of DOPO-grafted graphene oxide was mixed with 120 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 11.3 g of epoxidized triphosphazene was added, and the mixture was reacted at 150 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered and washed successively with N,N-dimethylformamide, ethanol, and water. The precipitate was then dried at 50 °C for 24 h to obtain the flame retardant. Step (3): Wash the polyester-cotton fabric with ethanol and water at room temperature, and dry it at 80°C for 5 minutes to obtain the pretreated polyester-cotton fabric. Flame retardant was ultrasonically dispersed in water to prepare a finishing solution with a flame retardant dosage of 75 g / L. The pretreated polyester-cotton fabric was immersed in the finishing solution at room temperature with a liquor ratio of 1:30 and an immersion time of 30 min. The fabric was then dipped and rubbed twice with a pick-up rate of 70%. It was then pre-dried at 80°C for 5 min and baked at 150°C for 2 min to obtain the surface fabric and the inner fabric, respectively. Step (4): Mix the recycled polyester fiber, hollow polyester fiber, and ES fiber evenly, form a web using a dry web-forming method, and then reinforce it using a thermal bonding method to obtain a web with a basis weight of 100 g / m². 2 Recycled polyester flakes; The mass ratio of recycled polyester fiber, hollow polyester fiber, and ES fiber is 64:19:17; the fiber arrangement direction in the fiber web is cross-arranged; the dry web forming conditions are: conveying speed of 13m / s and web forming speed of 40m / s; the thermal bonding reinforcement method conditions are: reinforcement temperature of 180℃ and output temperature of 12m / s. Recycled polyester wadding is used as the middle layer fabric. The layers are aligned in the order of the outer layer fabric, the middle layer fabric, and the inner layer fabric, and then sewn together using a multi-layer fabric quilting machine to obtain a warm, layered composite fabric.

[0028] Example 5 This embodiment discloses a method for preparing a thermal insulating layered composite fabric, including the following steps: Step (1): Dissolve 17.38 g of hexachlorocyclotriphosphazene in 100 mL of 1,4-dioxane to obtain a hexachlorocyclotriphosphazene solution; add 100 mL of 1,4-dioxane and 30.36 g of triethylamine to 33.04 g of hydroquinone, stir and dissolve in a nitrogen atmosphere, heat to 80 °C, add the hexachlorocyclotriphosphazene solution dropwise at a rate of 2 seconds / drop, after the addition is complete, react at 80 °C for 12 h, after the reaction is complete, filter to remove triethylamine hydrochloride, concentrate by rotary evaporation, extract with ethyl acetate, take the organic phase, dry with anhydrous sodium sulfate, concentrate again by rotary evaporation, and dry at 50 °C for 12 h to obtain phenolized cyclotriphosphazene; 30g of phenolized cyclotriphosphazene and 200g of epichlorohydrin were mixed and reacted at 110℃ for 1h. After the reaction was completed, the temperature was lowered to 60℃ and 12g of 30wt% sodium hydroxide aqueous solution was added. The reaction was carried out at 60℃ for 2h. After the reaction was completed, the mixture was cooled to room temperature, filtered under reduced pressure, and the filtrate was collected. The mixture was concentrated by rotary evaporation and extracted with dichloromethane. The organic phase was collected, dried with anhydrous sodium sulfate, concentrated again by rotary evaporation, and dried at room temperature for 12h to obtain epoxidized cyclotriphosphazene. Step (2): Mix 0.5g of graphene oxide with 120mL of N,N-dimethylformamide, sonicate for 30min, add 20mL of N,N-dimethylformamide solution of maleic anhydride, react in a nitrogen atmosphere at 80℃ for 24h, after the reaction is completed, centrifuge to collect the precipitate, wash with ethanol, and dry at 50℃ for 12h to obtain maleic anhydride-grafted graphene oxide; The N,N-dimethylformamide solution of maleic anhydride was prepared by mixing 2g of maleic anhydride with 20mL of N,N-dimethylformamide. 0.5 g of maleic anhydride-grafted graphene oxide was mixed with 140 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 4.32 g of DOPO was added, and the mixture was reacted at 130 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered, washed with ethanol, and dried at 50 °C for 12 h to obtain DOPO-grafted graphene oxide. 0.5 g of DOPO-grafted graphene oxide was mixed with 120 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 11.3 g of epoxidized triphosphazene was added, and the mixture was reacted at 150 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered and washed successively with N,N-dimethylformamide, ethanol, and water. The precipitate was then dried at 50 °C for 24 h to obtain the flame retardant. Step (3): Wash the polyester-cotton fabric with ethanol and water at room temperature, and dry it at 80°C for 5 minutes to obtain the pretreated polyester-cotton fabric. Flame retardant was ultrasonically dispersed in water to prepare a finishing solution, with a flame retardant dosage of 100 g / L. The pretreated polyester-cotton fabric was immersed in the finishing solution at room temperature with a liquor ratio of 1:30 and an immersion time of 30 min. The fabric was then dipped and rubbed twice with a pick-up rate of 70%. It was pre-dried at 80°C for 5 min and then baked at 150°C for 2 min to obtain the surface fabric and the inner fabric, respectively. Step (4): Mix the recycled polyester fiber, hollow polyester fiber, and ES fiber evenly, form a web using a dry web-forming method, and then reinforce it using a thermal bonding method to obtain a web with a basis weight of 100 g / m². 2 Recycled polyester flakes; The mass ratio of recycled polyester fiber, hollow polyester fiber, and ES fiber is 62:20:18; the fiber arrangement direction in the fiber web is cross-arranged; the dry web forming conditions are: conveying speed of 13m / s and web forming speed of 40m / s; the thermal bonding reinforcement method conditions are: reinforcement temperature of 180℃ and output temperature of 12m / s. Recycled polyester wadding is used as the middle layer fabric. The layers are aligned in the order of the outer layer fabric, the middle layer fabric, and the inner layer fabric, and then sewn together using a multi-layer fabric quilting machine to obtain a warm, layered composite fabric.

[0029] Comparative Example 1 This comparative example discloses a method for preparing a thermal insulating layered composite fabric, comprising the following steps: Step (1): Mix 0.5g of graphene oxide with 120mL of N,N-dimethylformamide, sonicate for 30min, add 20mL of N,N-dimethylformamide solution of maleic anhydride, react in a nitrogen atmosphere at 80℃ for 24h, after the reaction is completed, centrifuge to collect the precipitate, wash with ethanol, and dry at 50℃ for 12h to obtain maleic anhydride-grafted graphene oxide; The N,N-dimethylformamide solution of maleic anhydride was prepared by mixing 2g of maleic anhydride with 20mL of N,N-dimethylformamide. 0.5 g of maleic anhydride-grafted graphene oxide was mixed with 140 mL of N,N-dimethylformamide and ultrasonically dispersed for 1 h. Then, 4.32 g of DOPO was added, and the mixture was reacted at 130 °C for 24 h under a nitrogen atmosphere. After the reaction was completed, the precipitate was filtered, washed with ethanol, and dried at 50 °C for 12 h to obtain DOPO-grafted graphene oxide. Step (2): Wash the polyester-cotton fabric with ethanol and water at room temperature, and dry it at 80°C for 5 minutes to obtain the pretreated polyester-cotton fabric. DOPO-grafted graphene oxide was ultrasonically dispersed in water to prepare a finishing solution, with the amount of DOPO-grafted graphene oxide being 50 g / L. The pretreated polyester-cotton fabric was immersed in the finishing solution at room temperature with a liquor ratio of 1:30 and an immersion time of 30 min. The fabric was then subjected to two dips and two nips with a nip-out rate of 70%. It was then pre-dried at 80°C for 5 min and baked at 150°C for 2 min to obtain the surface fabric and the inner fabric, respectively. Step (3): Mix recycled polyester fiber, hollow polyester fiber, and ES fiber evenly, form a web using a dry web-forming method, and then reinforce it using a thermal bonding method to obtain a web with a basis weight of 100 g / m². 2 Recycled polyester flakes; The mass ratio of recycled polyester fiber, hollow polyester fiber, and ES fiber is 70:16:14; the fiber arrangement direction in the web is cross-arranged; the dry web forming conditions are: conveying speed of 13m / s and web forming speed of 40m / s; the thermal bonding reinforcement conditions are: reinforcement temperature of 180℃ and output temperature of 12m / s. Recycled polyester wadding is used as the middle layer fabric. The layers are aligned in the order of the outer layer fabric, the middle layer fabric, and the inner layer fabric, and then sewn together using a multi-layer fabric quilting machine to obtain a warm, layered composite fabric.

[0030] Comparative Example 2 This comparative example discloses a method for preparing a thermal insulating layered composite fabric, comprising the following steps: Step (1): Dissolve 17.38 g of hexachlorocyclotriphosphazene in 100 mL of 1,4-dioxane to obtain a hexachlorocyclotriphosphazene solution; add 100 mL of 1,4-dioxane and 30.36 g of triethylamine to 33.04 g of hydroquinone, stir and dissolve in a nitrogen atmosphere, heat to 80 °C, add the hexachlorocyclotriphosphazene solution dropwise at a rate of 2 seconds / drop, after the addition is complete, react at 80 °C for 12 h, after the reaction is complete, filter to remove triethylamine hydrochloride, concentrate by rotary evaporation, extract with ethyl acetate, take the organic phase, dry with anhydrous sodium sulfate, concentrate again by rotary evaporation, and dry at 50 °C for 12 h to obtain phenolized cyclotriphosphazene; 30g of phenolized cyclotriphosphazene and 200g of epichlorohydrin were mixed and reacted at 110℃ for 1h. After the reaction was completed, the temperature was lowered to 60℃ and 12g of 30wt% sodium hydroxide aqueous solution was added. The reaction was carried out at 60℃ for 2h. After the reaction was completed, the mixture was cooled to room temperature, filtered under reduced pressure, and the filtrate was collected. The mixture was concentrated by rotary evaporation and extracted with dichloromethane. The organic phase was collected, dried with anhydrous sodium sulfate, concentrated again by rotary evaporation, and dried at room temperature for 12h to obtain epoxidized cyclotriphosphazene. Step (2): Wash the polyester-cotton fabric with ethanol and water at room temperature, and dry it at 80°C for 5 minutes to obtain the pretreated polyester-cotton fabric. Epoxidized triphosphazene was ultrasonically dispersed in water to prepare a finishing solution, with the amount of epoxidized triphosphazene being 50 g / L. The pretreated polyester-cotton fabric was immersed in the finishing solution at room temperature with a liquor ratio of 1:30 and an immersion time of 30 min. The fabric was then subjected to two dips and two nips with a pick-up rate of 70%. It was then pre-dried at 80°C for 5 min and baked at 150°C for 2 min to obtain the surface fabric and the inner fabric, respectively. Step (4): Mix the recycled polyester fiber, hollow polyester fiber, and ES fiber evenly, form a web using a dry web-forming method, and then reinforce it using a thermal bonding method to obtain a web with a basis weight of 100 g / m². 2 Recycled polyester flakes; The mass ratio of recycled polyester fiber, hollow polyester fiber, and ES fiber is 70:16:14; the fiber arrangement direction in the web is cross-arranged; the dry web forming conditions are: conveying speed of 13m / s and web forming speed of 40m / s; the thermal bonding reinforcement conditions are: reinforcement temperature of 180℃ and output temperature of 12m / s. Recycled polyester wadding is used as the middle layer fabric. The layers are aligned in the order of the outer layer fabric, the middle layer fabric, and the inner layer fabric, and then sewn together using a multi-layer fabric quilting machine to obtain a warm, layered composite fabric.

[0031] In the above embodiments and comparative examples: the diameter of the graphene oxide sheets is 10-30 μm, and the thickness is 1-3 nm; the polyester-cotton fabric is a woven plain weave polyester-cotton fabric with a polyester content of 50% and a cotton content of 50%, and a weight of 180 g / m². 2 The length of the recycled polyester fiber is 38 mm and the linear density is 3.3 dtex; the length of the hollow polyester fiber is 38 mm and the linear density is 4.0 dtex; the length of the ES fiber is 38 mm and the linear density is 3.3 dtex.

[0032] Test case The performance of the thermal insulating layered composite fabrics prepared in Examples 1-5 and Comparative Examples 1-2 was tested, and the specific test results are shown in Table 1: Table 1

[0033] The tests for each indicator in Table 1 were conducted according to the following standards: The thermal insulation rate was determined according to GB / T 11048-1989 "Test Method for Thermal Insulation Performance of Textiles"; the far-infrared heating performance was expressed by temperature difference, and the test method was as follows: the thermal insulation layered composite fabrics prepared in Examples 1-5 and Comparative Examples 1-2 were placed on a heat-insulating platform, and a 500W infrared heating lamp was used to heat the fabric at a distance of 30cm for 5 minutes. The surface temperature difference of the fabric before and after heating was measured; the limiting oxygen index was tested according to GB / T 5454-1997 "Test Method for Combustion Performance of Textiles - Oxygen Index Method" for the surface layer fabrics prepared in Examples 1-5 and Comparative Examples 1-2.

[0034] Comparative Example 1 did not contain cyclotriphosphazene epoxide, resulting in reduced interfacial bonding between DOPO-grafted graphene oxide and the fabric surface. Consequently, after multiple washes, the flame retardant easily detached from the fabric surface, leading to a decrease in flame retardant performance with increasing wash cycles. Furthermore, the lack of cyclotriphosphazene's flame-retardant enhancement effect resulted in overall lower flame retardant performance compared to the Example.

[0035] Comparative Example 2 did not add DOPO-grafted graphene oxide. Although cyclotriphosphazene epoxide has good flame retardant properties, the far-infrared heating performance of the fabric is reduced because the finishing solution lacks graphene oxide, a component that can efficiently absorb and convert infrared radiation. Furthermore, when cyclotriphosphazene epoxide is used alone as a flame retardant, its flame retardant efficiency is lower than that of its combination with DOPO-grafted graphene oxide, resulting in a lower flame retardant performance of the fabric compared to the example.

[0036] It should be noted that the embodiments described above are only for explaining the present invention and do not constitute any limitation on the present invention. The present invention has been described with reference to typical embodiments, but it should be understood that the words used therein are descriptive and explanatory terms, not limiting terms. Modifications can be made to the present invention within the scope of the claims, and revisions can be made to the present invention without departing from the scope and spirit of the present invention. Although the present invention described herein relates to specific methods, materials, and embodiments, it does not mean that the present invention is limited to the specific examples disclosed herein; on the contrary, the present invention can be extended to all other methods and applications with the same function.

Claims

1. A method for preparing a thermally insulating layered composite fabric, characterized in that, Includes the following steps: Step (1): Mix DOPO-grafted graphene oxide with N,N-dimethylformamide, disperse by ultrasonication, add epoxidized triphosphazene, react, filter, wash, and dry to obtain flame retardant; Step (2): Disperse the flame retardant in water using ultrasound to prepare a finishing solution; wash and dry the polyester-cotton fabric, then immerse it in the finishing solution and bake it to obtain the surface fabric and the inner fabric, respectively. Step (3): Use recycled polyester wadding as the middle layer fabric, and combine it in the order of surface fabric, middle layer fabric and inner layer fabric to obtain a thermal layered composite fabric.

2. The method for preparing a thermal insulating layered composite fabric according to claim 1, characterized in that, The DOPO-grafted graphene oxide in step (1) is prepared by the following steps: S1. Mix graphene oxide with N,N-dimethylformamide, disperse by ultrasonication, add a solution of maleic anhydride in N,N-dimethylformamide, react, centrifuge, wash, and dry to obtain maleic anhydride-grafted graphene oxide. S2. Maleic anhydride-grafted graphene oxide is mixed with N,N-dimethylformamide, ultrasonically dispersed, DOPO is added, and the reaction is carried out. After the reaction is completed, the mixture is filtered, washed, and dried to obtain DOPO-grafted graphene oxide.

3. The method for preparing a thermal insulating layered composite fabric according to claim 1, characterized in that, In step (1), when preparing DOPO-grafted graphene oxide, in S1: the N,N-dimethylformamide solution of maleic anhydride is prepared by mixing 2g of maleic anhydride with 20mL of N,N-dimethylformamide; the ratio of graphene oxide, N,N-dimethylformamide, and the N,N-dimethylformamide solution of maleic anhydride is 0.5g:100-120mL:15-30mL; the reaction conditions are: reaction at 70-90℃ for 20-30h in a nitrogen atmosphere; In S2, the ratio of maleic anhydride-grafted graphene oxide, N,N-dimethylformamide, and DOPO is 0.5g:100-150mL:4.3-4.5g. The reaction conditions are: reaction at 120-130℃ for 24-28h under a nitrogen atmosphere.

4. The method for preparing a thermal insulating layered composite fabric according to claim 1, characterized in that, The epoxidized cyclotriphosphazene in step (1) is prepared by the following steps: S1. Add 1,4-dioxane and triethylamine sequentially to hydroquinone, stir to dissolve, add hexachlorocyclotriphosphazene solution dropwise, react, and after the reaction is completed, purify to obtain phenolized cyclotriphosphazene. S2. Phenolicized cyclotriphosphazene and epichlorohydrin are mixed and reacted. After the reaction is completed, the mixture is cooled, and an aqueous solution of sodium hydroxide is added to continue the reaction. After the reaction is completed, the mixture is purified to obtain epoxidized cyclotriphosphazene.

5. The method for preparing a thermal insulating layered composite fabric according to claim 1, characterized in that, In step (1), when preparing epoxidized triphosphazene, the ratio of hydroquinone, hexachlorocyclotriphosphazene, 1,4-dioxane, and triethylamine in S1 is 33-34:17-18:100-120mL:30-32g; the hexachlorocyclotriphosphazene solution is prepared by mixing hexachlorocyclotriphosphazene and 1,4-dioxane at a ratio of 17-18g:100mL; the dropping conditions of the hexachlorocyclotriphosphazene solution are: heating to 70-80℃ in a nitrogen atmosphere and dropping at a rate of 1-2 seconds / drop; the reaction conditions are: reacting at 70-80℃ in a nitrogen atmosphere for 12-14 hours. In S2, the ratio of phenolized triphosphazene, epichlorohydrin, and 30wt% sodium hydroxide aqueous solution is 20-30g: 180-220g: 10-12g; the reaction conditions are: react at 100-115℃ for 1h; the reaction is continued at 50-60℃ for 2-3h.

6. The method for preparing a thermal insulating layered composite fabric according to claim 1, characterized in that, In step (1), the ratio of DOPO-grafted graphene oxide, N,N-dimethylformamide, and epoxidized triphosphazene is 0.5g:100-140mL:10-15g; the reaction conditions are: reaction at 130-160℃ for 18-32h in a nitrogen atmosphere.

7. The method for preparing a thermal insulating layered composite fabric according to claim 1, characterized in that, In step (2): the amount of flame retardant in the finishing liquid is 50-100g / L; the impregnation conditions are: a bath ratio of 1:30-50, impregnation at room temperature for 30-50min, two dips and two rolls, and a roll residue of 70-80%; the baking conditions are: pre-baking at 70-90℃ for 3-5min, and baking at 130-180℃ for 1-3min.

8. The method for preparing a thermal insulating layered composite fabric according to claim 1, characterized in that, In step (3), the recycled polyester wadding is prepared by the following steps: Recycled polyester fiber, hollow polyester fiber, and ES fiber are mixed evenly and made into a fiber web by dry web forming. Then, the web is reinforced by thermal bonding to obtain recycled polyester wadding. The mass ratio of recycled polyester fiber, hollow polyester fiber, and ES fiber is 62-70:16-20:14-18; the fiber arrangement direction in the web is cross-arranged; the dry web forming conditions are: conveying speed of 13-15 m / s and web forming speed of 35-40 m / s; the thermal bonding reinforcement conditions are: reinforcement temperature of 150-180℃ and output temperature of 12-15 m / s; the basis weight of the recycled polyester wadding is 100-130 g / m². 2 .

9. A lightweight thermal insulation layered composite fabric prepared by the method for preparing thermal insulation layered composite fabric as described in any one of claims 1-8.

10. The application of the lightweight thermal insulating layered composite fabric as described in claim 9 in aircraft cabin quilts.

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