CN117512986B - Fire-retardant polyester fabric and preparation process thereof - Google Patents
Fire-retardant polyester fabric and preparation process thereofInfo
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- CN117512986B CN117512986B CN202311639623.9A CN202311639623A CN117512986B CN 117512986 B CN117512986 B CN 117512986B CN 202311639623 A CN202311639623 A CN 202311639623A CN 117512986 B CN117512986 B CN 117512986B
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/51—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/53—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with sulfur, selenium, tellurium, polonium or compounds thereof with hydrogen sulfide or its salts; with polysulfides
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
- D06M15/568—Reaction products of isocyanates with polyethers
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/22—Polymers or copolymers of halogenated mono-olefins
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/32—Polyesters
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/01—Stain or soil resistance
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/30—Flame or heat resistance, fire retardancy properties
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- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
本发明涉及纺织面料领域，具体是一种防火阻燃的涤纶面料及其制备工艺，选用聚乙烯醇、改性杂化二硫化钼、海藻酸钠静电纺丝制备阻燃纤维，将阻燃纤维与涤纶纤维混织后进行浸渍整理，选用改性杂化二硫化钼、自修复水性聚氨酯乳液制备防护整理液；用碳纳米管、十六烷基三甲基溴化铵、四水合钼酸铵、硫脲生成杂化二硫化钼，在杂化二硫化钼表面沉积苝四甲酸酐，然后接枝甲基硅酸三羟甲基甲胺笼状酯；在自修复水性聚氨酯乳液的制备中，选用含有多重氢键的2‑氨基‑5‑(2‑羟乙基)‑6‑甲基嘧啶‑4‑醇与聚四氢呋喃、异佛尔酮二异氰酸酯制备预聚体，引入双(2‑羟乙基)二硫化物作为扩链剂，引入甲基硅酸三羟甲基甲胺笼状酯、全氟聚醚醇作为封端剂。The invention relates to the field of textile fabrics, in particular to a fire-resistant and flame-retardant polyester fabric and a preparation process thereof. The invention comprises the following steps: polyvinyl alcohol, modified hybrid molybdenum disulfide and sodium alginate are selected for electrostatic spinning to prepare flame-retardant fibers; the flame-retardant fibers are blended with polyester fibers and then subjected to impregnation finishing; the modified hybrid molybdenum disulfide and a self-repairing waterborne polyurethane emulsion are selected for preparing a protective finishing liquid; carbon nanotubes, hexadecyltrimethylammonium bromide, ammonium molybdate tetrahydrate and thiourea are used to generate hybrid molybdenum disulfide; perylenetetracarboxylic anhydride is deposited on the surface of the hybrid molybdenum disulfide; and tris(hydroxymethyl)methylammonium caged ester of methylsilicate is grafted thereon; and in the preparation of the self-repairing waterborne polyurethane emulsion, 2-amino-5-(2-hydroxyethyl)-6-methylpyrimidine-4-ol containing multiple hydrogen bonds is selected for preparing a prepolymer with polytetrahydrofuran and isophorone diisocyanate; bis(2-hydroxyethyl) disulfide is introduced as a chain extender; and tris(hydroxymethyl)methylammonium caged ester of methylsilicate and perfluoropolyether alcohol are introduced as end-capping agents.
Description
Technical Field
The invention relates to the field of textile fabrics, in particular to a fireproof flame-retardant polyester fabric and a preparation process thereof.
Background
Polyester is a main kind of chemical fiber, the annual output of the polyester can be more than half of the total amount of the synthetic fiber, and the chemical component is polyethylene terephthalate, so the polyester is widely applied to various fields of automobiles, industry, clothing and the like due to the characteristics of high strength, good wear resistance, good elasticity and the like.
But the terylene fabric has poor flame retardant property, can generate a large amount of dense smoke and molten drops during combustion, and is easy to cause serious harm, thereby restricting the application of terylene. In order to improve the flame retardant property of the polyester fabric in the existing market, the flame retardant finishing agent or the auxiliary agent for the polyester fabric is generally finished, but the strength of the flame retardant finishing agent or the auxiliary agent is greatly damaged when the functional finishing is carried out, so that the flame retardant finishing agent has great significance in the aspects of protection, multifunction and the like of the polyester product.
Disclosure of Invention
The invention aims to provide a fireproof flame-retardant polyester fabric and a preparation process thereof, so as to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
A preparation process of fireproof flame-retardant polyester fabric comprises the following steps:
S1, preparing an electrostatic spinning solution by using polyvinyl alcohol, modified hybridized molybdenum disulfide, sodium alginate and deionized water, and performing electrostatic spinning to obtain flame-retardant fibers;
s2, blending and weaving the flame-retardant fibers and the polyester fibers to obtain a polyester composite fabric;
S3, preparing protective finishing liquid by using modified hybridized molybdenum disulfide and self-repairing aqueous polyurethane emulsion;
s4, soaking and rolling the terylene composite fabric in the protective finishing liquid for two times, and then pre-baking and baking to obtain the fireproof flame-retardant terylene fabric.
Further, the working condition of the electrostatic spinning is that the advancing speed of the electrostatic spinning solution is 0.8mL/h, the receiving distance is 15cm, the voltage is 23kV, and the temperature is 18-25 ℃.
Further, the working conditions of the two-soaking and two-rolling are that the soaking time is 10-20min, the rolling surplus rate is 75-80%, the pre-baking working conditions are that the temperature is kept at 75-80 ℃ for 3-5min, and the baking working conditions are that the temperature is kept at 110-120 ℃ for 10-12min.
Further, the mass ratio of the polyvinyl alcohol, the sodium alginate and the modified hybrid molybdenum disulfide in the electrostatic spinning solution is 4:2:1.
Further, the blending ratio of the flame retardant fiber to the polyester fiber in the polyester composite fabric is 50:50.
Further, the mass ratio of the modified hybrid molybdenum disulfide to the self-repairing aqueous polyurethane emulsion in the protective impregnating solution is 4-5%.
Further, the preparation of the self-repairing aqueous polyurethane emulsion comprises the following steps:
1) Mixing guanidine carbonate, 2-acetyl-gamma-butyrolactone, ethanol and triethylamine, preserving heat for 10-12h at 75-80 ℃, filtering, washing and drying to obtain 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidin-4-ol;
2) Under the nitrogen atmosphere, the polytetrahydrofuran is kept at 110 ℃ for 1-2 hours, isophorone diisocyanate, 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidine-4-alcohol, N-dimethylacetamide and dibutyltin dilaurate are added, the temperature is raised to 90-95 ℃ for 1-2 hours, bis (2-hydroxyethyl) disulfide is added, the temperature is lowered to 40-45 ℃, 1-2 hours is kept, trimethylol methylamine methylsilicate cage ester is added after the temperature is lowered to 35-40 ℃, the heat is kept for 1-2 hours, perfluoropolyether alcohol is added for 1-2 hours, methanol is added after the temperature is lowered to 18-25 ℃, the mixture is steamed in a spinning mode, deionized water is added for emulsification, and the self-repairing aqueous polyurethane emulsion with the mass fraction of 40-50% is prepared.
Further, the preparation of the modified hybrid molybdenum disulfide comprises the following steps:
(1) Mixing carbon nano tube, hexadecyl trimethyl ammonium bromide, ammonium molybdate tetrahydrate, thiourea and deionized water, performing ultrasonic dispersion for 10-15min, transferring into a hydrothermal kettle, preserving heat for 9-10h at 168-172 ℃, cooling, centrifuging, washing and drying to obtain hybridized molybdenum disulfide;
(2) Mixing the hybridized molybdenum disulfide and isopropanol, adding a mixed solution of perylene tetracarboxylic anhydride, chloroform and deionized water, and carrying out ultrasonic treatment for 15-20min to obtain composite molybdenum disulfide;
(3) Under the protection of nitrogen, mixing methyl silicate trimethylol methylamine cage ester and dimethyl sulfoxide, adding mixed solution of composite molybdenum disulfide, imidazole and acetone, heating to 115-120 ℃, preserving heat for 5-6 hours, cooling, adding absolute ethyl alcohol, centrifuging, washing and drying to obtain the modified hybrid molybdenum disulfide.
Further, the preparation of the trimethylol methylamine cage-like ester of methyl silicate comprises the following steps of mixing trimethylol aminomethane hydrochloride, triethylamine and dioxane under the protection of nitrogen, adding methyl trichlorosilane, preserving heat for 20-30min at 35-40 ℃, heating to 68-72 ℃ and preserving heat for 6-7h, filtering while the mixture is hot, adding deionized water, regulating the pH value to 7.9-8.1 by using triethylamine, filtering and washing to obtain the trimethylol methylamine cage-like ester of methyl silicate.
The invention has the beneficial effects that:
The invention provides a fireproof flame-retardant polyester fabric and a preparation process thereof, wherein polyvinyl alcohol, modified hybridized molybdenum disulfide and sodium alginate are selected for electrostatic spinning to prepare flame-retardant fibers, and (3) carrying out dipping finishing after mixing the flame-retardant fibers and the polyester fibers to prepare the fireproof flame-retardant polyester fabric with the self-repairing super-hydrophobic surface.
In order to improve the flame retardance and the environmental protection of the fabric, degradable raw materials such as sodium alginate and polyvinyl alcohol are selected for electrostatic spinning to prepare flame-retardant fibers, and in order to improve the toughness and the flame retardance of the flame-retardant fibers, modified hybridized molybdenum disulfide is selected as a toughening agent and a flame retardant.
The preparation method comprises the steps of generating hybridized molybdenum disulfide by using a carbon nano tube, cetyl trimethyl ammonium bromide, ammonium molybdate tetrahydrate and thiourea, depositing perylene tetracarboxylic anhydride on the surface of the hybridized molybdenum disulfide by using strong interaction of perylene tetracarboxylic anhydride and molybdenum disulfide, synthesizing methyl silicate trimethylol methylamine cage-shaped ester with flame retardance by using tris (hydroxymethyl) aminomethane hydrochloride, triethylamine, dioxane and methyl trichlorosilane to improve the flame retardance, and grafting methyl silicate trimethylol methylamine cage-shaped ester on the hybridized molybdenum disulfide by using anhydride in perylene tetracarboxylic anhydride on the hybridized molybdenum disulfide to react with amino-anhydride in the methyl silicate trimethylol methylamine cage-shaped ester to obtain halogen-free flame retardant modified hybridized molybdenum disulfide.
In order to endow the fabric with excellent mechanical damage resistance, the fabric is endowed with normal-temperature self-repairing property, modified hybridized molybdenum disulfide and self-repairing aqueous polyurethane emulsion are selected to prepare protective finishing liquid, in the preparation of the self-repairing aqueous polyurethane emulsion, 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidine-4-ol containing multiple hydrogen bonds, polytetrahydrofuran and isophorone diisocyanate are selected to prepare prepolymer, bis (2-hydroxyethyl) disulfide is introduced as a chain extender, trimethylol methylamine cage ester of methyl silicate and perfluoropolyether alcohol are introduced as a blocking agent, fluorine-containing aqueous self-repairing polyurethane containing multiple hydrogen bonds and dynamic disulfide bonds is synthesized, deionized water is used for emulsification, the self-repairing aqueous polyurethane emulsion is obtained, then modified hybridized molybdenum disulfide is added as a toughening agent and a flame retardant of the protective finishing liquid, and the mass ratio of the toughening agent and the flame retardant is controlled, so that the self-cleaning property of the fabric with the self-repairing super-hydrophobic surface is greatly improved, and the lasting flame-retardant effect is achieved.
Detailed Description
In the following, a technical solution in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In addition, if directional indications such as up, down, left, right, front, and rear are involved in the embodiment of the present invention, the directional indications are merely used to explain the relative positional relationship between the components, the movement condition, and the like in a certain specific posture, and if the specific posture is changed, the directional indications are changed accordingly. In addition, the technical solutions of the embodiments may be combined with each other, but it is necessary to base that the technical solutions can be realized by those skilled in the art, and when the technical solutions are contradictory or cannot be realized, the combination of the technical solutions should be considered to be absent and not within the scope of protection claimed in the present invention.
The following description of the embodiments of the present invention will be presented in further detail with reference to the examples, which should be understood as being merely illustrative of the present invention and not limiting.
Example 1A preparation process of fireproof flame-retardant polyester fabric comprises the following steps:
S1, preparing an electrostatic spinning solution by using polyvinyl alcohol, modified hybridized molybdenum disulfide, sodium alginate and deionized water, and preparing flame-retardant fibers by electrostatic spinning;
The working condition of the electrostatic spinning is that the advancing speed of the electrostatic spinning solution is 0.8mL/h, the receiving distance is 15cm, the voltage is 23kV, and the temperature is 18 ℃;
Mixing 4g of polyvinyl alcohol and 400mL of deionized water, heating to 65 ℃, stirring until the mixture is dissolved, adding a mixed solution of 2g of sodium alginate and 100mL of deionized water, vacuumizing and standing for 7 hours, adding a mixed solution of 1g of modified hybrid molybdenum disulfide and 100mL of deionized water, and performing ultrasonic dispersion for 1 hour to obtain a spinning solution;
The preparation method of the modified hybridized molybdenum disulfide comprises the following steps:
(1) Mixing 2.4g of carbon nano tube, 0.8g of hexadecyl trimethyl ammonium bromide, 1.6g of ammonium molybdate tetrahydrate, 1.6g of thiourea and 200mL of deionized water, performing ultrasonic dispersion for 10min, transferring into a hydrothermal kettle, preserving heat for 10h at 168 ℃, cooling, centrifuging, washing and drying to obtain hybridized molybdenum disulfide;
(2) Mixing 50mg of hybridized molybdenum disulfide and 100mL of isopropanol, adding a mixed solution of 21.4mL of perylene tetracarboxylic anhydride, 100mg of chloroform and 100mL of deionized water, and carrying out ultrasonic treatment for 15min to obtain composite molybdenum disulfide;
(3) Under the protection of nitrogen, mixing 0.36g of methyl silicate trimethylol methylamine cage ester and 8mL of dimethyl sulfoxide, adding a mixed solution of 1g of composite molybdenum disulfide, 2g of imidazole and 3mL of acetone, heating to 115 ℃, preserving heat for 6 hours, cooling, adding 30mL of absolute ethyl alcohol, centrifuging, washing and drying to obtain modified hybrid molybdenum disulfide;
Under the protection of nitrogen, mixing 15.2g of tris (hydroxymethyl) aminomethane hydrochloride, 12.9g of triethylamine and 125mL of dioxane, adding 21.5g of methyltrichlorosilane, preserving heat for 30min at 35 ℃, heating to 68 ℃ and preserving heat for 7h, filtering while hot, adding 10mL of deionized water, regulating the pH value to 7.9 by using triethylamine, filtering and washing to obtain the tris (hydroxymethyl) aminomethane cage methyl silicate;
s2, blending and weaving the flame-retardant fibers and the polyester fibers to obtain a polyester composite fabric;
the blending ratio of the flame retardant fibers to the polyester fibers in the polyester composite fabric is 50:50;
S3, preparing protective finishing liquid by using modified hybridized molybdenum disulfide and self-repairing aqueous polyurethane emulsion;
The mass ratio of the modified hybridized molybdenum disulfide to the self-repairing aqueous polyurethane emulsion in the protective impregnating solution is 4%;
the preparation of the self-repairing aqueous polyurethane emulsion comprises the following steps:
1) 9.9g of guanidine carbonate, 7.2g of 2-acetyl-gamma-butyrolactone, 60mL of ethanol and 15mL of triethylamine are mixed, the mixture is kept at 75 ℃ for 12 hours, and the mixture is filtered, washed and dried to obtain 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidin-4-ol;
2) Under nitrogen atmosphere, 7g of polytetrahydrofuran is kept at 110 ℃ for 1h, 6.8g of isophorone diisocyanate, 1.5g of 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidine-4-ol, 3.5mLN, N-dimethylacetamide and 35mg of dibutyltin dilaurate are added, the temperature is raised to 90 ℃ for 2h, 0.8g of bis (2-hydroxyethyl) disulfide is added when the temperature is lowered to 45 ℃, the temperature is kept for 1h, 0.6g of trimethylol methylamine methylsilicate cage ester is added after the temperature is lowered to 40 ℃, the temperature is kept for 1h, 0.25g of perfluoropolyether alcohol is added for 1h, the temperature is lowered to 18 ℃ and 1mL of methanol is added, the mixture is subjected to rotary evaporation, deionized water is added for emulsification at 2500rpm, and the self-repairing aqueous polyurethane emulsion with the mass fraction of 40% is prepared;
S4, soaking and rolling the terylene composite fabric in protective finishing liquid for two times, and then pre-drying and baking to obtain the fireproof flame-retardant terylene fabric, wherein the working conditions of the soaking and rolling for two times are 10 minutes, the rolling surplus rate is 75%, the pre-drying working conditions are that the temperature is kept at 75 ℃ for 5 minutes, and the baking working conditions are that the temperature is kept at 110 ℃ for 12 minutes.
Example 2A preparation process of fireproof flame-retardant polyester fabric comprises the following steps:
S1, preparing an electrostatic spinning solution by using polyvinyl alcohol, modified hybridized molybdenum disulfide, sodium alginate and deionized water, and preparing flame-retardant fibers by electrostatic spinning;
the working condition of the electrostatic spinning is that the advancing speed of the electrostatic spinning solution is 0.8mL/h, the receiving distance is 15cm, the voltage is 23kV, and the temperature is 20 ℃;
Mixing 4g of polyvinyl alcohol and 400mL of deionized water, heating to 68 ℃, stirring until the mixture is dissolved, adding a mixed solution of 2g of sodium alginate and 100mL of deionized water, vacuumizing and standing for 7.5 hours, adding a mixed solution of 1g of modified hybrid molybdenum disulfide and 100mL of deionized water, and performing ultrasonic dispersion for 1.5 hours to obtain a spinning solution;
The preparation method of the modified hybridized molybdenum disulfide comprises the following steps:
(1) Mixing 2.4g of carbon nano tube, 0.8g of hexadecyl trimethyl ammonium bromide, 1.6g of ammonium molybdate tetrahydrate, 1.6g of thiourea and 200mL of deionized water, performing ultrasonic dispersion for 12min, transferring into a hydrothermal kettle, preserving heat for 9.5h at 170 ℃, cooling, centrifuging, washing and drying to obtain hybridized molybdenum disulfide;
(2) Mixing 50mg of hybridized molybdenum disulfide and 100mL of isopropanol, adding a mixed solution of 21.4mL of perylene tetracarboxylic anhydride, 100mg of chloroform and 100mL of deionized water, and carrying out ultrasonic treatment for 18min to obtain composite molybdenum disulfide;
(3) Under the protection of nitrogen, mixing 0.36g of methyl silicate trimethylol methylamine cage ester and 8mL of dimethyl sulfoxide, adding a mixed solution of 1g of composite molybdenum disulfide, 2g of imidazole and 3mL of acetone, heating to 118 ℃, preserving heat for 5.5 hours, cooling, adding 30mL of absolute ethyl alcohol, centrifuging, washing and drying to obtain modified hybrid molybdenum disulfide;
under the protection of nitrogen, mixing 15.2g of tris (hydroxymethyl) aminomethane hydrochloride, 12.9g of triethylamine and 125mL of dioxane, adding 21.5g of methyltrichlorosilane, preserving heat for 25min at 38 ℃, heating to 70 ℃ and preserving heat for 6.5h, filtering while hot, adding 10mL of deionized water, regulating the pH value to 8 with triethylamine, filtering and washing to obtain the tris (hydroxymethyl) aminomethane cage methyl silicate;
s2, blending and weaving the flame-retardant fibers and the polyester fibers to obtain a polyester composite fabric;
the blending ratio of the flame retardant fibers to the polyester fibers in the polyester composite fabric is 50:50;
S3, preparing protective finishing liquid by using modified hybridized molybdenum disulfide and self-repairing aqueous polyurethane emulsion;
the mass ratio of the modified hybridized molybdenum disulfide in the protective impregnating solution to the self-repairing aqueous polyurethane emulsion is 4.5%;
the preparation of the self-repairing aqueous polyurethane emulsion comprises the following steps:
1) 9.9g of guanidine carbonate, 7.2g of 2-acetyl-gamma-butyrolactone, 60mL of ethanol and 15mL of triethylamine are mixed, the mixture is kept at 78 ℃ for 11 hours, and the mixture is filtered, washed and dried to obtain 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidin-4-ol;
2) Under nitrogen atmosphere, 7g of polytetrahydrofuran is kept at 110 ℃ for 1.5 hours, 6.8g of isophorone diisocyanate, 1.5g of 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidine-4-ol, 3.5mLN, N-dimethylacetamide and 35mg of dibutyltin dilaurate are added, the temperature is raised to 92 ℃ for 1.5 hours, the temperature is reduced to 45 ℃ and 0.8g of bis (2-hydroxyethyl) disulfide is added, the temperature is kept for 1.5 hours, 0.6g of trimethylol methylamine cage methyl silicate is added after the temperature is reduced to 40 ℃, the temperature is kept for 1.5 hours, 0.25g of perfluoropolyether alcohol is added and kept for 1.5 hours, the temperature is reduced to 20 ℃ and 1mL of methanol is added, the mixture is subjected to rotary evaporation, deionized water is added for emulsification at the rotating speed of 2500rpm, and the self-repairing aqueous polyurethane emulsion with the mass fraction of 45% is prepared;
S4, soaking and rolling the terylene composite fabric in protective finishing liquid for two times, and then pre-drying and baking to obtain the fireproof flame-retardant terylene fabric, wherein the working conditions of the soaking and rolling for two times are 15min, the rolling surplus rate is 78%, the pre-drying working conditions are that the temperature is kept at 78 ℃ for 4min, and the baking working conditions are that the temperature is kept at 115 ℃ for 11min.
Example 3A preparation process of fireproof flame-retardant polyester fabric comprises the following steps:
S1, preparing an electrostatic spinning solution by using polyvinyl alcohol, modified hybridized molybdenum disulfide, sodium alginate and deionized water, and preparing flame-retardant fibers by electrostatic spinning;
the working condition of the electrostatic spinning is that the advancing speed of the electrostatic spinning solution is 0.8mL/h, the receiving distance is 15cm, the voltage is 23kV, and the temperature is 25 ℃;
Mixing 4g of polyvinyl alcohol and 400mL of deionized water, heating to 70 ℃, stirring until the mixture is dissolved, adding a mixed solution of 2g of sodium alginate and 100mL of deionized water, vacuumizing and standing for 8 hours, adding a mixed solution of 1g of modified hybrid molybdenum disulfide and 100mL of deionized water, and performing ultrasonic dispersion for 2 hours to obtain a spinning solution;
The preparation method of the modified hybridized molybdenum disulfide comprises the following steps:
(1) Mixing 2.4g of carbon nano tube, 0.8g of hexadecyl trimethyl ammonium bromide, 1.6g of ammonium molybdate tetrahydrate, 1.6g of thiourea and 200mL of deionized water, performing ultrasonic dispersion for 15min, transferring into a hydrothermal kettle, preserving heat for 9h at 172 ℃, cooling, centrifuging, washing and drying to obtain hybridized molybdenum disulfide;
(2) Mixing 50mg of hybridized molybdenum disulfide and 100mL of isopropanol, adding a mixed solution of 21.4mL of perylene tetracarboxylic anhydride, 100mg of chloroform and 100mL of deionized water, and carrying out ultrasonic treatment for 20min to obtain composite molybdenum disulfide;
(3) Under the protection of nitrogen, mixing 0.36g of methyl silicate trimethylol methylamine cage ester and 8mL of dimethyl sulfoxide, adding a mixed solution of 1g of composite molybdenum disulfide, 2g of imidazole and 3mL of acetone, heating to 120 ℃, preserving heat for 5 hours, cooling, adding 30mL of absolute ethyl alcohol, centrifuging, washing and drying to obtain modified hybrid molybdenum disulfide;
Under the protection of nitrogen, mixing 15.2g of tris (hydroxymethyl) aminomethane hydrochloride, 12.9g of triethylamine and 125mL of dioxane, adding 21.5g of methyltrichlorosilane, preserving heat for 20min at 40 ℃, heating to 72 ℃ and preserving heat for 6h, filtering while hot, adding 10mL of deionized water, regulating the pH value to 8.1 by using triethylamine, filtering and washing to obtain the tris (hydroxymethyl) aminomethane cage methyl silicate;
s2, blending and weaving the flame-retardant fibers and the polyester fibers to obtain a polyester composite fabric;
the blending ratio of the flame retardant fibers to the polyester fibers in the polyester composite fabric is 50:50;
S3, preparing protective finishing liquid by using modified hybridized molybdenum disulfide and self-repairing aqueous polyurethane emulsion;
the mass ratio of the modified hybridized molybdenum disulfide to the self-repairing aqueous polyurethane emulsion in the protective impregnating solution is 5%;
the preparation of the self-repairing aqueous polyurethane emulsion comprises the following steps:
1) 9.9g of guanidine carbonate, 7.2g of 2-acetyl-gamma-butyrolactone, 60mL of ethanol and 15mL of triethylamine are mixed, the mixture is kept at 75 to 80 ℃ for 10 to 12 hours, and the mixture is filtered, washed and dried to obtain 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidin-4-ol;
2) Under nitrogen atmosphere, 7g of polytetrahydrofuran is kept at 110 ℃ for 1-2h, 6.8g of isophorone diisocyanate, 1.5g of 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidine-4-ol, 3.5mLN, N-dimethylacetamide and 35mg of dibutyltin dilaurate are added, the temperature is raised to 90-95 ℃ for 1-2h, the temperature is lowered to 45 ℃ and 0.8g of bis (2-hydroxyethyl) disulfide is added, the temperature is kept for 2h, 0.6g of trimethylol methylamine methylsilicate cage ester is added after the temperature is lowered to 40 ℃, the temperature is kept for 2h, 0.25g of perfluoropolyether alcohol is added and kept for 2h, the temperature is lowered to 25 ℃ and 1mL of methanol is added, the mixture is distilled, deionized water is added for emulsification at the rotating speed of 2500rpm, and the self-repairing aqueous polyurethane emulsion with the mass fraction of 50% is prepared;
S4, soaking and rolling the terylene composite fabric in protective finishing liquid for two times, and then pre-drying and baking to obtain the fireproof flame-retardant terylene fabric, wherein the working conditions of the soaking and rolling for two times are 20 minutes, the rolling surplus rate is 80%, the pre-drying working conditions are that the temperature is kept at 80 ℃ for 3 minutes, and the baking working conditions are that the temperature is kept at 120 ℃ for 10 minutes.
Comparative example 1. With example 3 as the control, no trimethylol methylamine methylsilicate cage was prepared and the other procedures were normal.
Comparative example 2 Using example 3 as a control group, molybdenum disulfide (M104968: arabia Ding Shiji) was used instead of the modified hybrid molybdenum disulfide, and the other procedures were normal.
Comparative example 3 Using example 3 as a control group, the modified hybrid molybdenum disulfide was replaced with carbon nanotubes, and the other procedures were normal.
Comparative example 4 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidin-4-ol was not prepared by using example 3 as a control group, and the other procedures were normal.
Comparative example 5 Using example 3 as a control, no perfluoropolyether alcohol was added and the other procedure was normal.
The thickness of the terylene composite fabric in the examples and the comparative examples is 1mm, and the thickness of the protective finishing liquid formed on the terylene composite fabric is 100 mu m.
The raw material sources are as follows:
Polyester fiber (0.89 dtex x 38 mm): seisakusho chemical raw materials Co., ltd, perfluoro polyether alcohol 90317-77-4: henan Weitakoshi chemical technology Co., ltd, polyvinyl alcohol P139545, sodium alginate S100128, carbon nanotube C313046, cetyl trimethyl ammonium bromide H108983, ammonium molybdate tetrahydrate A116375, thiourea T112512, perylene tetracarboxylic anhydride P121510, dimethyl sulfoxide D103272, imidazole I108707, tris (hydroxymethyl) aminomethane hydrochloride T431526, triethylamine T103285, dioxane D116157, methyl trichlorosilane M104828, guanidine carbonate G104710, 2-acetyl-gamma-butyrolactone A108065, polytetrahydrofuran P118599, isophorone diisocyanate I109582, N-dimethylacetamide D108096, dibutyl tin dilaurate D100274, bis (2-hydroxyethyl) disulfide B598951: arabian Ding Shiji, isopropanol, chloroform, acetone, anhydrous ethanol, methanol, and reagent for analysis of medicine groups.
Performance test:
Cutting into 30cm×5cm, testing warp breaking strength with reference to GB/T3923.1-2013, characterizing water contact angle, testing with 4 μl deionized water drop, limiting oxygen index with reference to ASTMD2863-08, cutting sample to 5×15cm, washing sample with standard water for 20 times and 25 deg.C for 20min before measurement, self-repairing by marking scratch with length of 100 μm, width of 20 μm and depth of 100 μm on the surface of sample, maintaining temperature at 25deg.C for 12h, observing scratch length with electron microscope, characterizing self-repairing rate, and self-repairing rate= (1-L/L 0)×100％,l0 is initial scratch length, L is scratch length after heat preservation, as shown in Table 1;
TABLE 1
| Breaking strength (N) | Water contact angle (°) | Limiting oxygen index | Self-repair rate (%) | |
| Example 1 | 600.7 | 155 | 42 | 99.8 |
| Example 2 | 601.4 | 155 | 43 | 99.9 |
| Example 3 | 602.9 | 156 | 44 | 100 |
| Comparative example 1 | 497.6 | 153 | 31 | 99.7 |
| Comparative example 2 | 472.3 | 149 | 28 | 96.5 |
| Comparative example 3 | 483.5 | 148 | 29 | 95.8 |
| Comparative example 4 | / | 150 | 37 | 89.4 |
| Comparative example 5 | / | 132 | 36 | 99.6 |
The fabric prepared in the embodiment 1-3 of the invention has the warp breaking strength of 600.7-602.9N, the water contact angle of 155-156 degrees, the limiting oxygen index of 42-44 and the self-repairing rate of 99.8-100 percent, which shows that the polyester fabric prepared according to the invention is a fireproof flame-retardant polyester fabric with a self-repairing superhydrophobic surface, and the items in the table/the table show are not tested.
Comparing example 3 with comparative example 1, the grafting of trimethylol methylamine methylsilicate cage-like ester on the hybrid molybdenum disulfide is beneficial to improving the flame retardance of the fabric.
By comparing the example 3 with the comparative example 2 and the comparative example 3, the mechanical strength and the flame retardance of the fabric can be effectively improved by adding the modified hybrid molybdenum disulfide into the flame-retardant fiber and the protective finishing liquid.
Comparing the embodiment 3 with the comparative example 4 and the comparative example 5, in the preparation of the self-repairing aqueous polyurethane emulsion, selecting 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidine-4-alcohol and polytetrahydrofuran, isophorone diisocyanate to prepare a prepolymer, introducing bis (2-hydroxyethyl) disulfide to serve as a chain extender, introducing methyl silicate trimethylol methylamine cage ester and perfluor polyether alcohol to serve as a blocking agent, synthesizing fluorine-containing aqueous self-repairing polyurethane containing multiple hydrogen bonds and dynamic disulfide bonds, emulsifying with deionized water to obtain the self-repairing aqueous polyurethane emulsion, adding modified hybridized molybdenum disulfide to serve as a toughening agent and a flame retardant of the protective finishing liquid, and then performing twice-soaking, pre-baking and baking treatment on the polyester composite fabric in the protective finishing liquid to obtain the fireproof flame-retardant polyester fabric with the self-repairing super-hydrophobic surface, thereby greatly improving the self-cleaning property of the fabric and achieving the lasting flame-retardant effect.
The foregoing description is only of the preferred embodiments of the present invention and is not intended to limit the scope of the invention, and all changes of the equivalent structure or direct/indirect application of the present invention in the related technical fields are included in the scope of the present invention under the inventive concept of the present invention.
Claims (7)
1. A preparation process of fireproof flame-retardant polyester fabric is characterized by comprising the following steps:
S1, preparing an electrostatic spinning solution by using polyvinyl alcohol, modified hybridized molybdenum disulfide, sodium alginate and deionized water, and performing electrostatic spinning to obtain flame-retardant fibers;
s2, blending and weaving the flame-retardant fibers and the polyester fibers to obtain a polyester composite fabric;
S3, preparing protective finishing liquid by using modified hybridized molybdenum disulfide and self-repairing aqueous polyurethane emulsion;
s4, soaking and rolling the terylene composite fabric in protective finishing liquid for two times, and then pre-baking and baking to obtain the fireproof flame-retardant terylene fabric;
the preparation of the self-repairing aqueous polyurethane emulsion comprises the following steps:
1) Mixing guanidine carbonate, 2-acetyl-gamma-butyrolactone, ethanol and triethylamine, preserving heat for 10-12h at 75-80 ℃, filtering, washing and drying to obtain 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidin-4-ol;
2) Under the nitrogen atmosphere, the polytetrahydrofuran is kept at 110 ℃ for 1-2 hours, isophorone diisocyanate, 2-amino-5- (2-hydroxyethyl) -6-methylpyrimidine-4-alcohol, N-dimethylacetamide and dibutyltin dilaurate are added, the temperature is raised to 90-95 ℃ for 1-2 hours, bis (2-hydroxyethyl) disulfide is added, the temperature is lowered to 40-45 ℃, 1-2 hours is kept, trimethylol methylamine methylsilicate cage ester is added after the temperature is lowered to 35-40 ℃, the heat is kept for 1-2 hours, perfluoropolyether alcohol is added for 1-2 hours, methanol is added after the temperature is lowered to 18-25 ℃, the mixture is steamed in a rotary mode, deionized water is added for emulsification, and the self-repairing aqueous polyurethane emulsion with the mass fraction of 40-50% is prepared;
The preparation method of the modified hybridized molybdenum disulfide comprises the following steps:
(1) Mixing carbon nano tube, hexadecyl trimethyl ammonium bromide, ammonium molybdate tetrahydrate, thiourea and deionized water, performing ultrasonic dispersion for 10-15min, transferring into a hydrothermal kettle, preserving heat for 9-10h at 168-172 ℃, cooling, centrifuging, washing and drying to obtain hybridized molybdenum disulfide;
(2) Mixing the hybridized molybdenum disulfide and isopropanol, adding a mixed solution of perylene tetracarboxylic anhydride, chloroform and deionized water, and carrying out ultrasonic treatment for 15-20min to obtain composite molybdenum disulfide;
(3) Under the protection of nitrogen, mixing methyl silicate trimethylol methylamine cage ester and dimethyl sulfoxide, adding mixed solution of composite molybdenum disulfide, imidazole and acetone, heating to 115-120 ℃, preserving heat for 5-6 hours, cooling, adding absolute ethyl alcohol, centrifuging, washing and drying to obtain modified hybrid molybdenum disulfide;
the preparation method of the methyl silicate trimethylol methylamine cage ester comprises the following steps of mixing the trimethylol aminomethane hydrochloride, triethylamine and dioxane under the protection of nitrogen, adding methyl trichlorosilane, preserving heat for 20-30min at 35-40 ℃, heating to 68-72 ℃ and preserving heat for 6-7h, filtering while the mixture is hot, adding deionized water, regulating the pH value to 7.9-8.1 by using triethylamine, filtering and washing to obtain the methyl silicate trimethylol methylamine cage ester.
2. The preparation process of the fireproof flame-retardant polyester fabric as claimed in claim 1, wherein the working condition of the electrostatic spinning is that the advancing speed of the electrostatic spinning solution is 0.8mL/h, the receiving distance is 15cm, the voltage is 23kV, and the temperature is 18-25 ℃.
3. The preparation process of the fireproof flame-retardant polyester fabric is characterized in that the working conditions of twice soaking and twice rolling are that the soaking time is 10-20min, the rolling surplus rate is 75-80%, the pre-baking working conditions are that the temperature is kept at 75-80 ℃ for 3-5min, and the baking working conditions are that the temperature is kept at 110-120 ℃ for 10-12min.
4. The preparation process of the fireproof flame-retardant polyester fabric, which is disclosed in claim 1, is characterized in that the mass ratio of polyvinyl alcohol, sodium alginate and modified hybrid molybdenum disulfide in the electrostatic spinning solution is 4:2:1.
5. The preparation process of the fireproof and flame-retardant polyester fabric as claimed in claim 1, wherein the blending ratio of the flame-retardant fibers to the polyester fibers in the polyester composite fabric is 50:50.
6. The preparation process of the fireproof flame-retardant polyester fabric, which is characterized in that the mass ratio of modified hybrid molybdenum disulfide to self-repairing aqueous polyurethane emulsion in the protective finishing liquid is 4-5%.
7. A fireproof flame-retardant polyester fabric is characterized by being prepared by the process of any one of claims 1-6.
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