CN115534453A - Efficient flame-retardant heat-insulation composite fabric and application thereof - Google Patents
Efficient flame-retardant heat-insulation composite fabric and application thereof Download PDFInfo
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- CN115534453A CN115534453A CN202211245810.4A CN202211245810A CN115534453A CN 115534453 A CN115534453 A CN 115534453A CN 202211245810 A CN202211245810 A CN 202211245810A CN 115534453 A CN115534453 A CN 115534453A
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- China
- Prior art keywords
- fiber
- flame
- retardant heat
- insulation
- calcium titanate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/14—Mixture of at least two fibres made of different materials
- B32B2262/152—Knitted fabric
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/304—Insulating
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/30—Properties of the layers or laminate having particular thermal properties
- B32B2307/306—Resistant to heat
- B32B2307/3065—Flame resistant or retardant, fire resistant or retardant
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
- B32B2307/51—Elastic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2307/00—Properties of the layers or laminate
- B32B2307/70—Other properties
- B32B2307/73—Hydrophobic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2437/00—Clothing
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- Engineering & Computer Science (AREA)
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Abstract
The invention discloses a high-efficiency flame-retardant heat-insulation composite fabric, which is obtained by compounding a flame-retardant heat-insulation protective layer arranged on an outer layer and a skin-friendly layer arranged on an inner layer; the flame-retardant heat-insulation protective layer comprises flame-retardant heat-insulation fibers which are modified polyimide fibers. The composite fabric capable of effectively retarding flame and insulating heat is prepared, can be used under conventional high-temperature conditions, and can have good usability even under harsh conditions. The composite fabric prepared by the invention comprises two layers of fabrics, wherein the outer layer is a flame-retardant high-temperature-resistant fabric layer, so that the composite fabric can play a role in blocking the external high-temperature environment and protecting a human body; the inner layer is a soft and skin-friendly fabric layer, and aims to make the skin of a human body more comfortable when contacting and more convenient for people to use.
Description
Technical Field
The invention relates to the field of fabrics, in particular to a high-efficiency flame-retardant heat-insulation composite fabric and application thereof.
Background
The flame-retardant heat-insulation fabric has wide application prospects in production and life, for example, heat-insulation gloves made of the flame-retardant heat-insulation fabric can be used for being taken out of containers placed in a microwave oven and an oven, and are also suitable for carrying pot handles, plates, pot covers and the like; in the industrial aspect, the flame-retardant heat-insulating fabric can be applied to the manufacture of electronic equipment such as semiconductors, electronics, precision instruments, integrated circuits, liquid crystal displays and the like, and the high-temperature environment in the industries such as biological pharmacy, optical instruments, food and the like.
Especially in the field of electric welding and fire control, the requirement to thermal-insulated surface fabric is quite high, still must prevent that open flame from causing the injury to the wearer when having thermal-insulated, and some surface fabrics only have thermal-insulated function and can not fire-retardant or possess fire-retardant function but can not insulate against heat, have great threat to the personal safety of wearer. In addition, some heat-insulating and flame-retardant fabrics are very thick and heavy, and in the fields of ovens, electric welding and fire fighting, the actions of wearers are greatly limited by clothes and protective articles made of the thick and heavy fabrics, and the hands are not flexible enough when the clothes and protective articles are used, so that the safety is reduced.
The polyimide fiber is a high-performance organic fiber developed in recent years, has a glass transition temperature of more than 400 ℃, a thermal decomposition temperature of more than 550 ℃ and a low thermal conductivity coefficient, belongs to a self-extinguishing polymer, is very suitable for being used as a flame-retardant and heat-insulating fabric material, is not alkali-resistant and hot-steam-resistant, and is easy to be subjected to alkali and superheated steam actionHydrolysis, and in addition, as the demand increases, the properties of polyimide also need to be improved. However, polyimide has a long molecular chain, a compact structure, poor processability, poor cross-linking with other materials, and poor modification binding property with other materials. For example, patent application No. CN201710857569.3 discloses a polyimide/titanium dioxide hybrid fiber using nano TiO 2 4,4' -diaminodiphenyl ether and pyromellitic dianhydride are mixed and reacted to prepare the polyimide/titanium dioxide hybrid fiber, and although the strength is improved, the nano TiO is 2 In a physical doping manner, the fiber is not firm after long-term application, and the performance of the fiber is further influenced.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a high-efficiency flame-retardant heat-insulation composite fabric and application thereof.
The purpose of the invention is realized by adopting the following technical scheme:
the first purpose of the invention is to provide a high-efficiency flame-retardant heat-insulation composite fabric, which is obtained by compounding a flame-retardant heat-insulation protective layer arranged on an outer layer and a skin-friendly layer arranged on an inner layer; the flame-retardant heat-insulation protective layer comprises flame-retardant heat-insulation fibers, wherein the flame-retardant heat-insulation fibers are modified polyimide fibers.
Preferably, the compounding mode of the flame-retardant heat-insulation protective layer and the skin-friendly layer comprises any one of a glue bonding method, a suture sewing method and a double-sided adhesive lining method.
Preferably, the flame-retardant heat-insulation protective layer is woven by taking flame-retardant heat-insulation fibers and spandex fibers as raw materials, wherein the mass ratio of the flame-retardant heat-insulation fibers is 95.7-98.6%, and the mass ratio of the spandex fibers is 1.4-5.3%.
Preferably, the skin-friendly layer is a fabric formed by weaving chemical fibers and/or natural fibers serving as raw materials; the weaving pattern includes knitting or tatting.
Preferably, the natural fibers include at least one of plant fibers, animal fibers, and mineral fibers; the plant fiber comprises at least one of cotton fiber and hemp fiber; the animal fiber comprises at least one of wool fiber, cashmere fiber, camel hair fiber, rabbit hair fiber and cattle hair fiber; the mineral fiber is asbestos fiber.
Preferably, the chemical fibers include rayon and synthetic fibers; the artificial fiber comprises at least one of viscose fiber, dadu fiber, acetate fiber, peanut fiber, glass fiber, carbon fiber, chitin fiber and seaweed gel fiber; the synthetic fiber includes at least one of polyester fiber, polyamide fiber, polyacrylonitrile fiber, polyvinyl alcohol fiber, polyvinyl chloride fiber, polypropylene fiber, and polyurethane fiber.
Preferably, the preparation method of the flame-retardant heat-insulating fiber comprises the following steps:
(1) Treating copper calcium titanate powder by using amino functional group silane to obtain aminated copper calcium titanate powder; adding terephthalaldehyde and tetrahydropyrrole for reaction treatment to prepare aldehyde copper calcium titanate powder;
(2) Reacting biphenyl tetracarboxylic dianhydride with hydrazine hydrate to prepare an imide monomer;
(3) Reacting and combining the prepared imide monomer and the aldehyde copper calcium titanate powder in a solution to obtain a modified mixed solution;
(4) The flame-retardant heat-insulating fiber is prepared by synthesizing a polyamic acid solution in a solution by using biphenyl tetracarboxylic dianhydride and p-phenylenediamine as basic reactants, adding a modified mixed solution, mixing to form a spinning solution, and performing wet spinning treatment and high-temperature treatment.
More preferably, the preparation method of the flame-retardant heat-insulating fiber comprises the following steps:
s1, weighing copper calcium titanate powder (CaCu) 3 Ti 4 O 12 ) Mixing the calcium salt with absolute ethyl alcohol into a flask, ultrasonically dispersing for 2-4h, adding amino functional group silane, stirring in a water bath for 20-30h, centrifugally collecting powder, washing with ultrapure water and ethanol for three times respectively, and vacuum drying to obtain aminated copper calcium titanate powder; wherein, the particle size of the copper calcium titanate powder is 100-200nm, and the mass ratio of the copper calcium titanate powder, the amino functional group silane and the absolute ethyl alcohol is 1;
s2, weighing aminated copper calcium titanate powder and absolute ethyl alcohol, mixing the aminated copper calcium titanate powder and the absolute ethyl alcohol into a flask to form a mixed solution, weighing terephthalaldehyde and tetrahydropyrrole under the protection of nitrogen, sequentially adding the terephthalaldehyde and the tetrahydropyrrole into the mixed solution, heating to 55-60 ℃, refluxing and stirring for 10-20h, naturally cooling to room temperature, centrifuging to obtain a powder material, washing with ethyl alcohol and dichloromethane for three times respectively, and performing vacuum drying to obtain aldehyde group copper calcium titanate powder; wherein, the mass ratio of the aminated copper calcium titanate powder to the absolute ethyl alcohol is 1-50, and the mass ratio of the terephthalaldehyde to the pyrrolidine to the mixed solution is 3.2-4.8;
s3, weighing biphenyl tetracarboxylic dianhydride and absolute ethyl alcohol, mixing in a flask, uniformly mixing at room temperature, introducing nitrogen as protective gas, and dropwise adding hydrazine hydrate (N) 2 H 4 ·H 2 O), heating to 70-80 ℃, refluxing and stirring for 2-4h under water bath condensation, centrifuging and collecting a precipitate, and performing vacuum drying treatment to obtain an imide monomer; wherein, the mass ratio of the biphenyl tetracarboxylic dianhydride to the hydrazine hydrate to the absolute ethyl alcohol is 1.24-1.36;
s4, adding an imide monomer into N, N-Dimethylformamide (DMF), heating to completely dissolve under the protection of nitrogen, gradually adding aldehyde copper calcium titanate powder under the stirring action, heating to 180-220 ℃ after adding, stirring for reacting for 10-20h, and naturally cooling to room temperature to obtain a modified mixed solution; wherein, the mass ratio of the imide monomer, the aldehyde copper calcium titanate powder and the N, N-dimethylformamide is 1;
s5, weighing biphenyl tetracarboxylic dianhydride, mixing with N, N-Dimethylformamide (DMF), adding p-phenylenediamine, and stirring at room temperature for 10-15 hours under the protection of nitrogen to obtain a polyamic acid solution; mixing the modified mixed solution with the polyamic acid solution, stirring at room temperature for 3-6h to obtain a modified polyamic acid spinning solution, and preparing the flame-retardant heat-insulating fiber through wet spinning treatment and high-temperature treatment; wherein, the mass ratio of the biphenyl tetracarboxylic dianhydride to the p-phenylenediamine to the N, N-dimethylformamide is 2.8-3.4; the mass ratio of the modified mixed solution to the polyamic acid solution is 1:2-5.
Preferably, the biphenyl tetracarboxylic dianhydride is 2,3,3',4' -biphenyl tetracarboxylic dianhydride or 3,3',4,4' -biphenyl tetracarboxylic dianhydride.
Preferably, the amino functional group silane is silane coupling agent KH-550 (gamma-aminopropyltriethoxysilane).
Preferably, the wet spinning process is as follows:
the modified polyimide spinning solution is defoamed in vacuum, placed in a spinning machine, sprayed out through a spinneret orifice, sequentially passes through an air layer and a coagulating bath, is coagulated into filaments, and is subjected to drafting, washing and rolling treatment to obtain the flame-retardant heat-insulating fiber; wherein the pore size of the spinneret orifice is 0.15-0.35mm, the spinneret speed is 4-6m/min, the air layer path is 20-30mm, the coagulating bath is formed by mixing DMF (dimethyl formamide) and deionized water according to the mass ratio of 2:8, the temperature of the coagulating bath is 10-15 ℃, and the drawing multiple is 2.2-2.5 times.
Preferably, the high-temperature treatment process is as follows:
the filamentous material obtained after wet spinning treatment is placed in a vacuum box, the temperature is raised to 100 ℃ at the speed of 5 ℃/min, the temperature is kept for 1h, then the temperature is raised to 300 ℃ at the speed of 5 ℃/min, and the temperature is kept for 1h respectively when the temperature is raised to 150 ℃, 200 ℃, 250 ℃ and 300 ℃.
Preferably, the weaving mode of the flame-retardant heat-insulation protective layer is plain weaving with staggered warps and wefts, the flame-retardant heat-insulation fibers and the spandex fibers are blended into warps and wefts, the density of the warps is 180-220 pieces/10 cm, the density of the wefts is 90-130 pieces/10 cm, and the thickness of the fabric is 0.5-1mm.
The second purpose of the invention is to provide the application of the high-efficiency flame-retardant heat-insulation composite fabric, and the high-efficiency flame-retardant heat-insulation composite fabric is applied to the fields of electric welding and fire fighting.
The invention has the beneficial effects that:
1. the composite fabric capable of effectively retarding flame and insulating heat is prepared, can be used under conventional high-temperature conditions, and can have good usability even under harsh conditions. The composite fabric prepared by the invention comprises two layers of fabrics, wherein the outer layer is a flame-retardant high-temperature-resistant fabric layer, so that the composite fabric can play a role in blocking the external high-temperature environment and protecting a human body; the inner layer is a soft and skin-friendly fabric layer, and aims to make the skin of a human body more comfortable when contacting and more convenient for people to use.
2. The flame-retardant high-temperature-resistant fabric layer on the outer layer of the fabric is mainly woven by taking flame-retardant high-temperature-resistant modified polyimide fibers (flame-retardant heat-insulating fibers) as raw materials, and a small amount of spandex fibers are added to improve the elasticity of the fabric to a certain extent. The modified polyimide fiber is modified by taking the polyimide fiber as a base material. Although the existing polyimide fiber has good high temperature resistance and heat insulation performance, the existing polyimide fiber is easy to hydrolyze under the action of alkali and superheated water vapor, a main chain in a molecule of the existing polyimide fiber has a plurality of polar groups, and the existing polyimide fiber is easy to absorb water in a humid environment, so that the existing polyimide fiber is used again under the high temperature condition after absorbing water to form the superheated water vapor to accelerate the hydrolysis. In the invention, a polyimide fiber fabric which is high temperature resistant, heat insulating, water repellent, light, thin and durable is synthesized in a special mode.
3. In the process of synthesizing the modified polyimide fiber, the nano-scale calcium copper titanate with a perovskite cubic crystal system structure is selected as a modified filler, the calcium copper titanate has a low thermal conductivity coefficient, very high stability and high dielectric constant at high temperature, and the strength, the insulativity and the high-temperature dimensional stability of the material can be enhanced. In the invention, the copper calcium titanate is subjected to surface treatment, ethanol is used for ultrasonic dispersion, then the copper calcium titanate is combined with aminosilane for amination, and then hydroformylation is carried out under the action of terephthalaldehyde and tetrahydropyrrole, so as to obtain the hydroformylation copper calcium titanate.
4. The modified polyimide fiber prepared by the invention is integrally characterized in that a modifier is added in the synthesis process of the traditional polyimide fiber, the modifier is obtained by reacting imide monomers containing terminal amino groups obtained by reacting biphenyl tetracarboxylic dianhydride with hydrazine hydrate (hydrazine hydrate) with aldehyde-based copper calcium titanate powder, and the amino groups and the aldehyde groups are condensed under proper conditions to form Schiff base structures so as to combine the copper calcium titanate with the imide monomers. In addition, the imide monomer in the modifier is synthesized by using the biphenyl tetracarboxylic dianhydride as a raw material, so the modifier has better compatibility with the polyamic acid and can exist in a system more uniformly and stably.
5. The modified polyimide fiber is prepared by using polyamic acid synthesized by biphenyl tetracarboxylic dianhydride and p-phenylenediamine as mother liquor, and adding a modifier synthesized by aldehyde copper calcium titanate powder and an imide monomer through wet spinning treatment and high-temperature treatment. The modified polyimide fiber is obtained by using biphenyl tetracarboxylic dianhydride and p-phenylenediamine as raw materials for synthesizing traditional polyamic acid, adding the modifier prepared by the invention, and then spinning and further performing staged high-temperature treatment, and has better mechanical property, hydrophobicity and stability.
Detailed Description
For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but are not to be construed as limiting the implementable scope of the present invention.
The invention is further described below with reference to the following examples.
Example 1
A high-efficiency flame-retardant heat-insulation composite fabric is obtained by compounding a flame-retardant heat-insulation protective layer arranged on an outer layer and a skin-friendly layer arranged on an inner layer; the flame-retardant heat-insulation protective layer comprises flame-retardant heat-insulation fibers which are modified polyimide fibers.
The skin-friendly layer is a fabric formed by weaving chemical fibers and/or natural fibers serving as raw materials; the weaving mode comprises knitting or tatting. The compounding mode of the flame-retardant heat-insulating protective layer and the skin-friendly layer comprises any one of a glue adhesion method, a suture line sewing method and a double-sided adhesive lining method.
The flame-retardant heat-insulation protective layer is formed by weaving flame-retardant heat-insulation fibers and spandex fibers serving as raw materials, wherein the mass percentage of the flame-retardant heat-insulation fibers is 96.8%, and the mass percentage of the spandex fibers is 3.2%. The weaving mode of the flame-retardant heat-insulation protective layer is plain weaving with staggered warps and wefts, the flame-retardant heat-insulation fibers and spandex fibers are blended into warps and wefts, the density of the warps is 200 pieces/10 cm, the density of the wefts is 110 pieces/10 cm, and the thickness of the fabric is 0.8mm.
The preparation method of the flame-retardant heat-insulating fiber comprises the following steps:
s1, weighing copper calcium titanate powder (CaCu) 3 Ti 4 O 12 ) Mixing the powder with absolute ethyl alcohol into a flask, performing ultrasonic dispersion for 3 hours, adding a silane coupling agent KH-550 (gamma-aminopropyltriethoxysilane), stirring in a water bath for 25 hours, centrifuging to collect the powder, washing with ultrapure water and ethanol for three times respectively, and performing vacuum drying to obtain aminated copper calcium titanate powder; wherein the particle size of the copper calcium titanate powder is 100-200nm, and the mass ratio of the copper calcium titanate powder to the amino functional group silane to the absolute ethyl alcohol is 1;
s2, weighing aminated copper calcium titanate powder and absolute ethyl alcohol, mixing the aminated copper calcium titanate powder and the absolute ethyl alcohol into a flask to form a mixed solution, weighing terephthalaldehyde and tetrahydropyrrole under the protection of nitrogen, sequentially adding the terephthalaldehyde and the tetrahydropyrrole into the mixed solution, heating to 55 ℃, refluxing and stirring for 15 hours, naturally cooling to room temperature, centrifuging to obtain a powder material, washing with ethyl alcohol and dichloromethane for three times respectively, and performing vacuum drying to obtain aldehyde-based copper calcium titanate powder; wherein, the mass ratio of the aminated copper calcium titanate powder to the absolute ethyl alcohol is 1;
s3, weighing 3,3',4,4' -biphenyl tetracarboxylic dianhydride and absolute ethyl alcohol, mixing in a flask, uniformly mixing at room temperature, introducing nitrogen as a protective gas, and dropwise adding hydrazine hydrate (N) 2 H 4 ·H 2 O), heating to 70 ℃, refluxing and stirring for 3 hours under water bath condensation, centrifugally collecting precipitate, and performing vacuum drying treatment to obtain an imide monomer; wherein, the mass ratio of 3,3',4,4' -biphenyl tetracarboxylic dianhydride, hydrazine hydrate and absolute ethyl alcohol is 1.28;
s4, adding an imide monomer into N, N-Dimethylformamide (DMF), heating to completely dissolve under the protection of nitrogen, gradually adding aldehyde copper calcium titanate powder under the stirring action, heating to 200 ℃ after adding, stirring for reacting for 10-20 hours, and naturally cooling to room temperature to obtain a modified mixed solution; wherein the mass ratio of the imide monomer, the aldehyde copper calcium titanate powder and the N, N-dimethylformamide is 1;
s5, weighing 3,3',4,4' -biphenyl tetracarboxylic dianhydride, mixing with N, N-Dimethylformamide (DMF), adding p-phenylenediamine, and stirring at room temperature for 10 hours under the protection of nitrogen to obtain a polyamic acid solution; mixing the modified mixed solution with the polyamic acid solution, stirring at room temperature for 4 hours again to obtain a modified polyamic acid spinning solution, and preparing the flame-retardant heat-insulating fiber through wet spinning treatment and high-temperature treatment; wherein the mass ratio of 3,3',4,4' -biphenyl tetracarboxylic dianhydride, p-phenylenediamine and N, N-dimethylformamide is 3.1; the mass ratio of the modified mixed solution to the polyamic acid solution was 1:4.
Wherein, the wet spinning process comprises the following steps:
the modified polyimide spinning solution is defoamed in vacuum, placed in a spinning machine, sprayed out through a spinneret orifice, sequentially passes through an air layer and a coagulating bath, is coagulated into filaments, and is subjected to drafting, washing and rolling treatment to obtain the flame-retardant heat-insulating fiber; wherein the pore diameter of the spinneret orifice is 0.25mm, the spinneret speed is 5m/min, the air layer path is 25mm, the coagulating bath is formed by mixing DMF (dimethyl formamide) and deionized water according to the mass ratio of 2:8, the temperature of the coagulating bath is 10 ℃, and the drawing multiple is 2.3 times.
Wherein the high-temperature treatment process comprises the following steps:
the filamentous material obtained after wet spinning treatment is placed in a vacuum box, the temperature is raised to 100 ℃ at the speed of 5 ℃/min, the temperature is kept for 1h, then the temperature is raised to 300 ℃ at the speed of 5 ℃/min, and the temperature is kept for 1h respectively when the temperature is raised to 150 ℃, 200 ℃, 250 ℃ and 300 ℃.
Example 2
A high-efficiency flame-retardant heat-insulation composite fabric is obtained by compounding a flame-retardant heat-insulation protective layer arranged on an outer layer and a skin-friendly layer arranged on an inner layer; the flame-retardant heat-insulation protective layer comprises flame-retardant heat-insulation fibers which are modified polyimide fibers.
The skin-friendly layer is a fabric formed by weaving chemical fibers and/or natural fibers serving as raw materials; the weaving mode comprises knitting or tatting. The compounding mode of the flame-retardant heat-insulating protective layer and the skin-friendly layer comprises any one of a glue adhesion method, a suture line sewing method and a double-sided adhesive lining method.
The flame-retardant heat-insulation protective layer is formed by weaving flame-retardant heat-insulation fibers and spandex fibers serving as raw materials, wherein the mass percentage of the flame-retardant heat-insulation fibers is 98.6%, and the mass percentage of the spandex fibers is 1.4%. The weaving mode of the flame-retardant heat-insulation protective layer is plain weaving with staggered warps and wefts, the flame-retardant heat-insulation fibers and spandex fibers are blended into warps and wefts, the density of the warps is 180 pieces/10 cm, the density of the wefts is 130 pieces/10 cm, and the thickness of the fabric is 0.5mm.
The preparation method of the flame-retardant heat-insulating fiber comprises the following steps:
s1, weighing copper calcium titanate powder (CaCu) 3 Ti 4 O 12 ) Mixing the powder with absolute ethyl alcohol into a flask, ultrasonically dispersing for 2 hours, adding a silane coupling agent KH-550 (gamma-aminopropyltriethoxysilane), stirring for 20 hours in a water bath, centrifugally collecting the powder, washing the powder for three times by using ultrapure water and ethanol respectively, and drying in vacuum to obtain aminated copper calcium titanate powder; wherein the particle size of the copper calcium titanate powder is 100-200nm, and the mass ratio of the copper calcium titanate powder to the amino functional group silane to the absolute ethyl alcohol is 1;
s2, weighing aminated copper calcium titanate powder and absolute ethyl alcohol, mixing the aminated copper calcium titanate powder and the absolute ethyl alcohol into a flask to form a mixed solution, weighing terephthalaldehyde and tetrahydropyrrole under the protection of nitrogen, sequentially adding the terephthalaldehyde and the tetrahydropyrrole into the mixed solution, heating to 55 ℃, refluxing and stirring for 10 hours, naturally cooling to room temperature, centrifuging to obtain a powder material, washing with ethyl alcohol and dichloromethane for three times respectively, and performing vacuum drying to obtain aldehyde-based copper calcium titanate powder; wherein, the mass ratio of the aminated copper calcium titanate powder to the absolute ethyl alcohol is 1;
s3, weighing 3,3',4,4' -biphenyl tetracarboxylic dianhydride and absolute ethyl alcohol, mixing in a flask, uniformly mixing at room temperature, introducing nitrogen as a protective gas, and dropwise adding hydrazine hydrate (N) 2 H 4 ·H 2 O), heating to 70 ℃, refluxing and stirring for 2 hours under water bath condensation, centrifugally collecting precipitate, and performing vacuum drying treatment to obtain an imide monomer; wherein, 3,3',4,4' -biphenyltetracarboxylic acidThe mass ratio of the acid dianhydride to the hydrazine hydrate to the absolute ethyl alcohol is 1;
s4, adding an imide monomer into N, N-Dimethylformamide (DMF), heating to completely dissolve under the protection of nitrogen, gradually adding aldehyde copper calcium titanate powder under the stirring action, heating to 180 ℃, stirring for reacting for 10 hours after the addition is finished, and naturally cooling to room temperature to obtain a modified mixed solution; wherein the mass ratio of the imide monomer, the aldehyde copper calcium titanate powder and the N, N-dimethylformamide is 1;
s5, weighing 3,3',4,4' -biphenyl tetracarboxylic dianhydride, mixing with N, N-Dimethylformamide (DMF), adding p-phenylenediamine, and stirring at room temperature for 10 hours under the protection of nitrogen to obtain a polyamic acid solution; mixing the modified mixed solution with the polyamic acid solution, stirring at room temperature for 3 hours again to obtain a modified polyamic acid spinning solution, and preparing the flame-retardant heat-insulating fiber through wet spinning treatment and high-temperature treatment; wherein, the mass ratio of 3,3',4,4' -biphenyl tetracarboxylic dianhydride, p-phenylenediamine and N, N-dimethylformamide is 2.8; the mass ratio of the modified mixed solution to the polyamic acid solution was 1:2.
Wherein, the wet spinning process comprises the following steps:
the modified polyimide spinning solution is defoamed in vacuum, placed in a spinning machine, sprayed out through a spinneret orifice, sequentially passes through an air layer and a coagulating bath, is coagulated into filaments, and is subjected to drafting, washing and rolling treatment to obtain the flame-retardant heat-insulating fiber; wherein the pore diameter of the spinneret orifice is 0.15mm, the spinneret speed is 4m/min, the air layer path is 20mm, the coagulating bath is formed by mixing DMF (dimethyl formamide) and deionized water according to the mass ratio of 2:8, the temperature of the coagulating bath is 10 ℃, and the drawing multiple is 2.2 times.
Wherein the high-temperature treatment process comprises the following steps:
the filamentous material obtained after wet spinning treatment is placed in a vacuum box, the temperature is raised to 100 ℃ at the speed of 5 ℃/min, the temperature is kept for 1h, then the temperature is raised to 300 ℃ at the speed of 5 ℃/min, and the temperature is kept for 1h respectively when the temperature is raised to 150 ℃, 200 ℃, 250 ℃ and 300 ℃.
Example 3
A high-efficiency flame-retardant heat-insulation composite fabric is obtained by compounding a flame-retardant heat-insulation protective layer arranged on an outer layer and a skin-friendly layer arranged on an inner layer; the flame-retardant heat-insulation protective layer comprises flame-retardant heat-insulation fibers, wherein the flame-retardant heat-insulation fibers are modified polyimide fibers.
The skin-friendly layer is a fabric formed by weaving chemical fibers and/or natural fibers serving as raw materials; the weaving mode comprises knitting or tatting. The compounding mode of the flame-retardant heat-insulating protective layer and the skin-friendly layer comprises any one of a glue adhesion method, a suture line sewing method and a double-sided adhesive lining method.
The flame-retardant heat-insulation protective layer is formed by weaving flame-retardant heat-insulation fibers and spandex fibers serving as raw materials, wherein the mass percentage of the flame-retardant heat-insulation fibers is 95.7%, and the mass percentage of the spandex fibers is 5.3%. The weaving mode of the flame-retardant heat-insulation protective layer is plain weaving with staggered warps and wefts, the flame-retardant heat-insulation fiber and the spandex fiber are blended into warps and wefts, the density of the warps is 220 pieces/10 cm, the density of the wefts is 90 pieces/10 cm, and the thickness of the fabric is 1mm.
The preparation method of the flame-retardant heat-insulation fiber comprises the following steps:
s1, weighing copper calcium titanate powder (CaCu) 3 Ti 4 O 12 ) Mixing the powder with absolute ethyl alcohol into a flask, ultrasonically dispersing for 4 hours, adding a silane coupling agent KH-550 (gamma-aminopropyltriethoxysilane), stirring for 30 hours in a water bath, centrifugally collecting the powder, washing the powder for three times by using ultrapure water and ethanol respectively, and drying in vacuum to obtain aminated copper calcium titanate powder; wherein the particle size of the copper calcium titanate powder is 100-200nm, and the mass ratio of the copper calcium titanate powder to the amino functional group silane to the absolute ethyl alcohol is 1;
s2, weighing aminated copper calcium titanate powder and absolute ethyl alcohol, mixing the aminated copper calcium titanate powder and the absolute ethyl alcohol into a flask to form a mixed solution, weighing terephthalaldehyde and tetrahydropyrrole under the protection of nitrogen, sequentially adding the terephthalaldehyde and the tetrahydropyrrole into the mixed solution, heating to 60 ℃, refluxing and stirring for 20 hours, naturally cooling to room temperature, centrifuging to obtain a powder material, washing with ethyl alcohol and dichloromethane for three times respectively, and performing vacuum drying to obtain aldehyde-based copper calcium titanate powder; wherein, the mass ratio of the aminated copper calcium titanate powder to the absolute ethyl alcohol is 1;
s3, weighing 3,3',4,4' -biphenyl tetracarboxylic dianhydride and absolute ethyl alcohol, mixing in a flask, uniformly mixing at room temperature, introducing nitrogen as a protective gas, and dropwise adding hydrazine hydrate (N) 2 H 4 ·H 2 O), heating to 80 ℃, refluxing and stirring for 4 hours under water bath condensation, centrifugally collecting precipitate, and performing vacuum drying treatment to obtain an imide monomer; wherein the mass ratio of 3,3',4,4' -biphenyl tetracarboxylic dianhydride, hydrazine hydrate and absolute ethyl alcohol is 1;
s4, adding an imide monomer into N, N-Dimethylformamide (DMF), heating to completely dissolve under the protection of nitrogen, gradually adding aldehyde copper calcium titanate powder under the stirring action, heating to 220 ℃, stirring for reacting for 20 hours after the addition is finished, and naturally cooling to room temperature to obtain a modified mixed solution; wherein the mass ratio of the imide monomer, the aldehyde copper calcium titanate powder and the N, N-dimethylformamide is 1;
s5, weighing 3,3',4,4' -biphenyl tetracarboxylic dianhydride, mixing with N, N-Dimethylformamide (DMF), adding p-phenylenediamine, and stirring at room temperature for 15 hours under the protection of nitrogen to obtain a polyamic acid solution; mixing the modified mixed solution with the polyamic acid solution, stirring for 6 hours at room temperature again to obtain a modified polyamic acid spinning solution, and preparing the flame-retardant heat-insulating fiber through wet spinning treatment and high-temperature treatment; wherein, the mass ratio of 3,3',4,4' -biphenyl tetracarboxylic dianhydride, p-phenylenediamine and N, N-dimethylformamide is 3.4; the mass ratio of the modified mixed solution to the polyamic acid solution was 1:5.
Wherein, the wet spinning process comprises the following steps:
the modified polyimide spinning solution is defoamed in vacuum, placed in a spinning machine, sprayed out through a spinneret orifice, sequentially passes through an air layer and a coagulating bath, is coagulated into filaments, and is subjected to drafting, washing and rolling treatment to obtain the flame-retardant heat-insulating fiber; wherein the pore diameter of the spinneret orifice is 0.35mm, the spinneret speed is 6m/min, the air layer path is 30mm, the coagulating bath is formed by mixing DMF (dimethyl formamide) and deionized water according to the mass ratio of 2:8, the temperature of the coagulating bath is 15 ℃, and the drawing multiple is 2.5 times.
Wherein the high-temperature treatment process comprises the following steps:
the filamentous material obtained after wet spinning treatment is placed in a vacuum box, the temperature is raised to 100 ℃ at the speed of 5 ℃/min, the temperature is kept for 1h, then the temperature is raised to 300 ℃ at the speed of 5 ℃/min, and the temperature is kept for 1h respectively when the temperature is raised to 150 ℃, 200 ℃, 250 ℃ and 300 ℃.
Comparative example 1
Compared with the fabric in the embodiment 1, the flame-retardant heat-insulation protective layer fabric is different in that the flame-retardant heat-insulation fibers are polyimide fibers. The fabric is woven by taking flame-retardant heat-insulation fibers and spandex fibers as raw materials, wherein the mass percentage of the flame-retardant heat-insulation fibers is 96.8%, and the mass percentage of the spandex fibers is 3.2%. The weaving mode of the flame-retardant heat-insulation protective layer is plain weaving with staggered warps and wefts, the flame-retardant heat-insulation fibers and spandex fibers are blended into warps and wefts, the density of the warps is 200 pieces/10 cm, the density of the wefts is 110 pieces/10 cm, and the thickness of the fabric is 0.8mm.
The flame-retardant heat-insulating fiber is a polyimide fiber and is synthesized by taking biphenyl tetracarboxylic dianhydride and p-phenylenediamine as raw materials, and the flame-retardant heat-insulating fiber comprises the following steps: weighing biphenyl tetracarboxylic dianhydride and N, N-Dimethylformamide (DMF), mixing, adding p-phenylenediamine, and stirring at room temperature for 10-15h under the protection of nitrogen to obtain a polyamic acid solution; carrying out wet spinning treatment and high-temperature treatment on the obtained polyamide acid spinning solution to prepare the flame-retardant heat-insulating fiber; wherein, the mass ratio of the biphenyl tetracarboxylic dianhydride to the p-phenylenediamine to the N, N-dimethylformamide is 2.8-3.4; the wet spinning process and the high temperature process were the same as in example 1.
Comparative example 2
Compared with the example 1, the flame-retardant heat-insulation protective layer fabric is different in the synthesis mode of flame-retardant heat-insulation fibers. The flame-retardant heat-insulating fiber is a modified polyimide fiber and is synthesized by the following steps:
s1, dispersing copper calcium titanate powder in N, N-dimethylformamide, and fully mixing to obtain a modified mixed solution; wherein the mass ratio of the calcium copper titanate powder to the N, N-dimethylformamide is 0.4;
s2, weighing 3,3',4,4' -biphenyl tetracarboxylic dianhydride, mixing with N, N-Dimethylformamide (DMF), adding p-phenylenediamine, and stirring at room temperature for 10 hours under the protection of nitrogen to obtain a polyamic acid solution; mixing the modified mixed solution with the polyamic acid solution, stirring at room temperature for 4 hours again to obtain a modified polyamic acid spinning solution, and preparing the flame-retardant heat-insulating fiber through wet spinning treatment and high-temperature treatment; wherein, the mass ratio of 3,3',4,4' -biphenyl tetracarboxylic dianhydride, p-phenylenediamine and N, N-dimethylformamide is 3.1; the mass ratio of the modified mixed solution to the polyamic acid solution was 1:4.
In order to more clearly illustrate the content of the present invention, the present invention performs performance evaluation tests on the fabrics of the flame-retardant and heat-insulating protective layers obtained in examples 1 to 3 and comparative examples 1 to 2. The detection method comprises the following steps: the detection standard of the tearing strength refers to GB/T3917.1. The flame retardant detection standard is referred to GB 8965.1; the hot droplet resistance is the molten metal splash impact resistance, the detection standard refers to GB/T17599, 15 droplets of metal droplets are detected within 1min, and the temperature rise condition of the inner side of the fabric is detected; thermal protection (for TPP) is referred to standard GB 8965.1.
The alkaline water heat treatment is to prepare 0.1mol/L sodium hydroxide solution, immerse the fabric in the sodium hydroxide solution, boil the fabric for 30min, take out the fabric, wash the fabric, dry the fabric and detect the tearing strength.
The results of the various tests are shown in table 1:
table 1 fabric performance test results
As can be seen from table 1, the flame-retardant heat-insulating fabric prepared in examples 1 to 3 has strong flame-retardant heat-insulating capability, stronger water repellency and better mechanical strength, and the strength is reduced by far less than that of the fabric prepared in comparative examples 1 to 2 even after the fabric is treated in a harsher hot alkali solution, which indicates that the water resistance and the alkali resistance of the fabric are improved; the anti-dripping property shows that when 15 drops of metal are dripped, the temperature rise of the examples 1 to 3 is less than 10K, which shows that the anti-dripping property is stronger; the thermal protection is also higher than that of the traditional fabric.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. The efficient flame-retardant heat-insulation composite fabric is characterized by being obtained by compounding a flame-retardant heat-insulation protective layer arranged on an outer layer and a skin-friendly layer arranged on an inner layer; the flame-retardant heat-insulation protective layer comprises a flame-retardant heat-insulation fiber, wherein the flame-retardant heat-insulation fiber is a modified polyimide fiber; the preparation method of the flame-retardant heat-insulating fiber comprises the following steps:
(1) Treating copper calcium titanate powder by using amino functional group silane to obtain aminated copper calcium titanate powder; adding terephthalaldehyde and tetrahydropyrrole for reaction treatment to prepare aldehyde copper calcium titanate powder;
(2) Reacting biphenyl tetracarboxylic dianhydride with hydrazine hydrate to prepare an imide monomer;
(3) Reacting and combining the prepared imide monomer and the aldehyde copper calcium titanate powder in a solution to obtain a modified mixed solution;
(4) The flame-retardant heat-insulating fiber is prepared by synthesizing a polyamic acid solution in a solution by using biphenyl tetracarboxylic dianhydride and p-phenylenediamine as basic reactants, adding a modified mixed solution, mixing to form a spinning solution, and performing wet spinning treatment and high-temperature treatment.
2. The efficient flame-retardant heat-insulation composite fabric as claimed in claim 1, wherein the compounding manner of the flame-retardant heat-insulation protective layer and the skin-friendly layer comprises any one of a glue bonding method, a suture stitching method and a double-sided adhesive lining method.
3. The efficient flame-retardant heat-insulation composite fabric according to claim 1, wherein the flame-retardant heat-insulation protective layer is woven by taking flame-retardant heat-insulation fibers and spandex fibers as raw materials, wherein the mass ratio of the flame-retardant heat-insulation fibers is 95.7-98.6%, and the mass ratio of the spandex fibers is 1.4-5.3%.
4. The efficient flame-retardant heat-insulation composite fabric as claimed in claim 1, wherein the skin-friendly layer is a fabric formed by weaving chemical fibers and/or natural fibers as raw materials; the weaving mode comprises knitting or tatting; the natural fiber comprises at least one of plant fiber, animal fiber and mineral fiber; the plant fiber comprises at least one of cotton fiber and hemp fiber; the animal fiber comprises at least one of wool fiber, cashmere fiber, camel hair fiber, rabbit hair fiber and cattle hair fiber; the mineral fiber is asbestos fiber; the chemical fibers comprise artificial fibers and synthetic fibers; the artificial fiber comprises at least one of viscose fiber, dadu fiber, acetate fiber, peanut fiber, glass fiber, carbon fiber, chitin fiber and seaweed gel fiber; the synthetic fiber includes at least one of polyester fiber, polyamide fiber, polyacrylonitrile fiber, polyvinyl alcohol fiber, polyvinyl chloride fiber, polypropylene fiber, and polyurethane fiber.
5. The efficient flame-retardant heat-insulation composite fabric according to claim 1, wherein the preparation process of the copper calcium titanate powder aldehyde in the preparation method (1) of the flame-retardant heat-insulation fiber comprises the following steps:
s1, weighing copper calcium titanate powder, mixing the copper calcium titanate powder with absolute ethyl alcohol into a flask, ultrasonically dispersing for 2-4h, adding amino functional group silane, stirring for 20-30h in a water bath, centrifugally collecting powder, washing with ultrapure water and ethyl alcohol for three times respectively, and performing vacuum drying to obtain aminated copper calcium titanate powder; wherein, the particle size of the copper calcium titanate powder is 100-200nm, and the mass ratio of the copper calcium titanate powder, the amino functional group silane and the absolute ethyl alcohol is 1;
s2, weighing aminated copper calcium titanate powder and absolute ethyl alcohol, mixing the aminated copper calcium titanate powder and the absolute ethyl alcohol into a flask to form a mixed solution, weighing terephthalaldehyde and tetrahydropyrrole under the protection of nitrogen, sequentially adding the terephthalaldehyde and the tetrahydropyrrole into the mixed solution, heating to 55-60 ℃, refluxing and stirring for 10-20h, naturally cooling to room temperature, centrifuging to obtain a powder material, washing with ethyl alcohol and dichloromethane for three times respectively, and performing vacuum drying to obtain aldehyde group copper calcium titanate powder; wherein, the mass ratio of the aminated copper calcium titanate powder to the absolute ethyl alcohol is 1-50, and the mass ratio of the terephthalaldehyde to the pyrrolidine to the mixed solution is 3.2-4.8.
6. The efficient flame-retardant heat-insulation composite fabric according to claim 1, wherein the preparation process of the imide monomer in the preparation method (2) of the flame-retardant heat-insulation fiber comprises the following steps:
s3, weighing biphenyl tetracarboxylic dianhydride and absolute ethyl alcohol, mixing the mixture in a flask, uniformly mixing the mixture at room temperature, introducing nitrogen as protective gas, dropwise adding hydrazine hydrate, heating to 70-80 ℃, carrying out reflux stirring for 2-4h under water bath condensation, centrifugally collecting precipitate, and carrying out vacuum drying treatment to obtain an imide monomer; wherein, the mass ratio of the biphenyl tetracarboxylic dianhydride to the hydrazine hydrate to the absolute ethyl alcohol is 1.24-1.36.
7. The efficient flame-retardant heat-insulation composite fabric according to claim 1, wherein the preparation process of the modified mixed solution in the preparation method (3) of the flame-retardant heat-insulation fiber comprises the following steps:
s4, adding an imide monomer into N, N-dimethylformamide, heating to completely dissolve under the protection of nitrogen, gradually adding aldehyde copper calcium titanate powder under the stirring action, heating to 180-220 ℃ after adding, stirring for reacting for 10-20h, and naturally cooling to room temperature to obtain a modified mixed solution; wherein the mass ratio of the imide monomer, the copper calcium titanate powder and the N, N-dimethylformamide is 1.
8. The efficient flame-retardant and heat-insulating composite fabric as claimed in claim 1, wherein the preparation process of the flame-retardant and heat-insulating fiber in step (4) comprises:
s5, weighing biphenyl tetracarboxylic dianhydride, mixing with N, N-dimethylformamide, adding p-phenylenediamine, and stirring at room temperature for 10-15 hours under the protection of nitrogen to obtain a polyamic acid solution; mixing the modified mixed solution with the polyamic acid solution, stirring at room temperature for 3-6h to obtain a modified polyamic acid spinning solution, and preparing the flame-retardant heat-insulating fiber through wet spinning treatment and high-temperature treatment; wherein, the mass ratio of the biphenyl tetracarboxylic dianhydride to the p-phenylenediamine to the N, N-dimethylformamide is 2.8-3.4; the mass ratio of the modified mixed solution to the polyamic acid solution is 1:2-5.
9. The efficient flame-retardant heat-insulation composite fabric according to claim 1, wherein the flame-retardant heat-insulation protective layer is woven by plain knitting with staggered warps and wefts, the flame-retardant heat-insulation fibers and the spandex fibers are blended into warps and wefts, the density of the warps is 180-220 pieces/10 cm, the density of the wefts is 90-130 pieces/10 cm, and the thickness of the fabric is 0.5-1mm.
10. The application of the high-efficiency flame-retardant heat-insulation composite fabric is characterized in that the high-efficiency flame-retardant heat-insulation composite fabric disclosed by any one of claims 1 to 9 is applied to the fields of electric welding and fire fighting.
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