CN119392504A - Environmentally friendly breathable polyester fabric and preparation process thereof - Google Patents

Environmentally friendly breathable polyester fabric and preparation process thereof Download PDF

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Publication number
CN119392504A
CN119392504A CN202411658422.8A CN202411658422A CN119392504A CN 119392504 A CN119392504 A CN 119392504A CN 202411658422 A CN202411658422 A CN 202411658422A CN 119392504 A CN119392504 A CN 119392504A
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epoxy
environmentally friendly
polyester fabric
solution
flame retardant
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黄明坤
马业俊
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Jiangsu Beltefu New Materials Co ltd
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Jiangsu Beltefu New Materials Co ltd
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Priority to CN202411658422.8A priority Critical patent/CN119392504A/en
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/37Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/564Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
    • D06M15/568Reaction products of isocyanates with polyethers
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/02Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
    • DTEXTILES; PAPER
    • D01NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01FCHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F8/00Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/18Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/208Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads cellulose-based
    • DTEXTILES; PAPER
    • D03WEAVING
    • D03DWOVEN FABRICS; METHODS OF WEAVING; LOOMS
    • D03D15/00Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
    • D03D15/20Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
    • D03D15/283Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads synthetic polymer-based, e.g. polyamide or polyester fibres
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/244Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus
    • D06M13/282Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing sulfur or phosphorus with compounds containing phosphorus
    • D06M13/292Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof
    • D06M13/298Mono-, di- or triesters of phosphoric or phosphorous acids; Salts thereof containing halogen atoms
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46Compounds containing quaternary nitrogen atoms
    • D06M13/461Quaternised amin-amides from polyamines or heterocyclic compounds or polyamino-acids
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/322Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing nitrogen
    • D06M13/46Compounds containing quaternary nitrogen atoms
    • D06M13/463Compounds containing quaternary nitrogen atoms derived from monoamines
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16Synthetic fibres, other than mineral fibres
    • D06M2101/30Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32Polyesters
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    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00Functionality of the treatment composition and/or properties imparted to the textile material
    • D06M2200/30Flame or heat resistance, fire retardancy properties
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product
    • Y02P70/62Manufacturing or production processes characterised by the final manufactured product related technologies for production or treatment of textile or flexible materials or products thereof, including footwear

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Abstract

本发明涉及面料制备技术领域,具体为一种环保透气型涤丝面料及其制备工艺。本发明以缩水甘油作为封端剂制备环氧基聚氨酯乳液;将丁香酚、二氯化磷酸苯酯为原料反应,以间氯过氧苯甲酸为氧化剂,制备环氧基阻燃剂;将N,N‑二乙基胺丙基甲基二甲氧基硅烷、环氧氯丙烷反应,得到环氧基有机硅季铵盐;将环氧基聚氨酯乳液、环氧基阻燃剂、环氧基有机硅季铵盐、固化剂混合并对涤丝改性;将羧甲基纤维素溶液和壳聚糖溶液的混合溶液通过静电纺丝技术制备生物基纺丝纤维,再与改性涤丝混纺得到涤丝面料。本发明制备的涤丝面料具有良好的阻燃性能、抗菌性能和透气性能,部分材料为可再生材料,经济环保,符合绿色发展需要。The present invention relates to the technical field of fabric preparation, specifically to an environmentally friendly breathable polyester fabric and a preparation process thereof. The present invention uses glycidol as a capping agent to prepare an epoxy polyurethane emulsion; uses eugenol and dichlorophenyl phosphate as raw materials for reaction, uses meta-chloroperbenzoic acid as an oxidant, and prepares an epoxy flame retardant; reacts N,N-diethylaminopropylmethyldimethoxysilane and epichlorohydrin to obtain an epoxy organosilicon quaternary ammonium salt; mixes the epoxy polyurethane emulsion, epoxy flame retardant, epoxy organosilicon quaternary ammonium salt, and a curing agent and modifies the polyester; prepares bio-based spinning fibers from a mixed solution of carboxymethyl cellulose solution and chitosan solution by electrostatic spinning technology, and then blends with modified polyester to obtain a polyester fabric. The polyester fabric prepared by the present invention has good flame retardant properties, antibacterial properties, and breathable properties, and some materials are renewable materials, which is economical and environmentally friendly, and meets the needs of green development.

Description

Environment-friendly breathable polyester yarn fabric and preparation process thereof
Technical Field
The invention relates to the technical field of fabric preparation, in particular to an environment-friendly breathable polyester yarn fabric and a preparation process thereof.
Background
The polyester filaments are also called polyester filaments, and are synthetic fibers. It is a synthetic fiber made up by using organic dibasic acid and dibasic alcohol through the process of chemical polycondensation, belonging to the category of macromolecular synthetic compound. Polyester has many advantages such as high strength, elastic recovery, chemical resistance, and the like. The clothing prepared from the polyester yarn fabric is firm and durable, can quickly recover the original shape, has excellent wrinkle resistance and shape retention in wearing, is not easy to wrinkle, and can keep the original shape of the clothing. In addition, the polyester yarn fabric has the characteristics of abrasion resistance, non-sticking hair and the like, so that the fabric looks tidier.
But the terylene material has the problems of poor air permeability, inflammability and the like, and is easy to breed germs, thereby causing diseases and affecting the health of people. In view of the above, it is highly desirable to provide a process for preparing an environment-friendly breathable polyester yarn fabric.
Disclosure of Invention
The invention aims to provide an environment-friendly breathable polyester yarn fabric and a preparation process thereof, so as to solve the problems in the background technology.
In order to solve the technical problems, the invention provides the following technical scheme that the environment-friendly breathable polyester yarn fabric and the preparation process thereof are as follows:
Step 1:
Washing and drying the polyester filaments, immersing the polyester filaments in the modifier according to a bath ratio of 1 (15-20) for 60-90 min, taking out, and vacuum drying at 80-90 ℃ for 3-5h to obtain modified polyester filaments;
step 2:
Dissolving carboxymethyl cellulose powder in deionized water to obtain carboxymethyl cellulose solution with the mass concentration of 10-15%, dissolving chitosan powder in acetic acid solution with the volume concentration of 2-3% to obtain chitosan solution with the mass fraction of 2-3%, mixing the carboxymethyl cellulose solution and the chitosan solution according to the volume ratio of (3-5) 1, adding glycerol with the total mass of 1-3% of the mixed solution, mixing in an oil bath at the temperature of 110-120 ℃ to obtain spinning solution, carrying out electrostatic spinning on the spinning solution to obtain bio-based spinning fibers, and blending the bio-based spinning fibers and modified polyester yarns to obtain a finished product.
Further, in the modifier, the contents of the components are calculated according to parts by weight, 100 parts of epoxy polyurethane emulsion, 5-8 parts of epoxy flame retardant, 10-14 parts of epoxy organosilicon quaternary ammonium salt and 20-24 parts of curing agent.
The preparation method of the epoxy polyurethane emulsion comprises the steps of mixing 35-50 parts of isophorone diisocyanate and 100 parts of polyethylene glycol 1000 according to parts by weight, reacting for 1-2 hours at 50-60 ℃ by taking dibutyl tin dilaurate as a catalyst, adding 6-8 parts of dimethylolpropionic acid to react for 0.5-1 hour, adding 5-7 parts of 1, 4-butanediol to react for 1-2 hours to obtain an isocyanate-terminated polyurethane prepolymer, adding glycidol according to the mol ratio of isocyanate groups to hydroxyl groups of 1:1 to react for 1-2 hours, cooling, adding 9-13 parts of triethylamine to neutralize, and adding deionized water to emulsify to obtain the epoxy polyurethane emulsion with the solid content of 30-40%.
Further, the preparation method of the epoxy-based flame retardant comprises the following steps:
S1, dispersing eugenol in ethyl acetate, cooling in an ice bath until the system temperature is stable by taking triethylamine as an acid binding agent, adding phenyl dichlorophosphate, stirring for 24 hours at 20-30 ℃, and finally separating, washing and rotary steaming the product to obtain phenyl di-eugenol phosphate;
And S2, dispersing phenyl diglucoside into ethyl acetate, stirring and adding m-chloroperoxybenzoic acid at 40-50 ℃ for reacting for 48-52 hours, separating liquid, washing, rotary steaming, cooling and recrystallizing the reaction product after the reaction is finished, and drying to obtain the epoxy flame retardant.
Further, in S1, eugenol and phenyl dichlorophosphate are reacted according to a molar ratio of 2:1.
Further, in S2, phenyl diglucoside and m-chloroperoxybenzoic acid react according to a molar ratio of 1:2.
The preparation method of the epoxy organosilicon quaternary ammonium salt comprises the steps of dispersing N, N-diethyl amine propyl methyl dimethoxy silane in absolute methanol under a nitrogen environment, heating to 55-65 ℃, adding a mixed solution of epichlorohydrin and absolute methanol, after the addition is finished, carrying out heat preservation reaction for 6-10 hours, carrying out rotary evaporation to remove the absolute methanol, eluting with absolute ethyl ether, and carrying out vacuum drying to obtain the epoxy organosilicon quaternary ammonium salt.
Further, N, N-diethyl amine propyl methyl dimethoxy silane and epoxy chloropropane are reacted according to the mol ratio of 1:1.
Further, in the environment-friendly breathable polyester yarn fabric, 15-20% of bio-based spinning fibers and 80-85% of modified polyester yarn are blended according to weight percentage.
Compared with the prior art, the polyester yarn fabric has the beneficial effects that the polyester yarn fabric prepared by the method has good flame retardant property, antibacterial property and air permeability, wherein part of the polyester yarn fabric is made of renewable environment-friendly materials, so that the preparation cost can be reduced, and the environment-friendly development requirement can be met.
The invention uses the modifier to modify the polyester yarn. The main components of the modifier include capping polyurethane prepolymer with glycidol as capping agent to obtain epoxy polyurethane emulsion, reacting eugenol with phenyl dichlorophosphate to obtain phenyl di-eugenol phosphate, epoxidizing double bonds at two ends of the phenyl di-eugenol phosphate with m-chloroperoxybenzoic acid as oxidant to obtain epoxy flame retardant, and reacting N, N-diethyl amine propyl methyl dimethoxy silane and epichlorohydrin as raw materials to obtain epoxy organosilicon quaternary ammonium salt. The main components contain epoxy groups, and a film layer can be formed on the surface of the polyester yarn after the epoxy groups are added and cured under the action of an amine curing agent, wherein the epoxy group flame retardant provides a certain flame retardant property, and the epoxy group organosilicon quaternary ammonium salt can not only enhance the antibacterial property of the surface of the polyester yarn, but also be an organosilicon cationic surfactant for application, and has the solubilization and emulsification effects on the modifier.
The invention blends polyester yarn and bio-based spinning fiber to prepare fabric, wherein the bio-based spinning fiber is obtained by mixing carboxymethyl cellulose solution and chitosan solution and then carrying out electrostatic spinning technology. In the bio-based spinning fiber, chitosan has good antibacterial performance, and the chitosan and the epoxy-based organosilicon quaternary ammonium salt in the modifier improve the antibacterial effect and the antibacterial durability together. The carboxymethyl cellulose and the chitosan are porous structure materials, so that the porous structure material has higher porosity and can improve the air permeability of the fabric. In addition, in the practical research and development process, the inventor surprisingly found that compared with the polyester yarn fabric modified by the modifier, the polyester yarn fabric disclosed by the invention has better flame retardant property, and through repeated researches, the inventor believes that the polyester yarn fabric mainly benefits from the existence of chitosan in the bio-based spinning fiber, the chitosan contains a large amount of amino groups, and the polyurethane coating on the surface of the modified polyester yarn is decomposed to generate isocyanate groups in the combustion process, and can react with the amino groups in the chitosan, so that the concentration of combustible substances is reduced, the combustion process is inhibited, and the flame retardant effect is further improved. It should be noted that the higher the amount of the bio-based spun fiber is, the better the amount is, and the higher the amount is, the crease resistance and rebound resilience of the fabric are reduced, so that the amount of the bio-based spun fiber and the modified polyester fiber is controlled during blending, specifically, 15-20% of the bio-based spun fiber and 80-85% of the modified polyester fiber are calculated according to weight percentages.
Detailed Description
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.
The polyester yarn is regenerated 150D polyester high stretch yarn DTY, comes from Zhejiang Huilong New Material Co., ltd., carboxymethyl cellulose comes from Hebei Yufei chemical Co., ltd., chitosan (deacetylation degree not less than 85%) comes from Shanxi blue grass biotechnology Co., ltd., and the curing agent is triethylene tetramine.
Example 1 an environment-friendly breathable polyester yarn fabric and a preparation process thereof, comprising the following steps:
Step 1:
s11, dispersing eugenol in ethyl acetate, cooling in an ice bath until the system temperature is stable by taking triethylamine as an acid binding agent, adding phenyl dichlorophosphate, stirring for 24 hours at 20 ℃, and finally separating, washing and rotary steaming the product to obtain phenyl di-eugenol phosphate, wherein eugenol and phenyl dichlorophosphate react according to a molar ratio of 2:1;
S12, dispersing phenyl diglucoside into ethyl acetate, stirring at 40 ℃ and adding m-chloroperoxybenzoic acid to react for 48 hours, separating liquid, washing, rotary steaming, cooling and recrystallizing a reaction product after the reaction is finished, and drying to obtain an epoxy flame retardant, wherein the phenyl diglucoside and the m-chloroperoxybenzoic acid react according to a molar ratio of 1:2;
step 2:
Dispersing N, N-diethyl amine propyl methyl dimethoxy silane in absolute methanol under the nitrogen environment, heating to 55 ℃, adding a mixed solution of epoxy chloropropane and absolute methanol, after the addition is finished, carrying out heat preservation reaction for 6 hours, removing the absolute methanol by rotary evaporation, eluting with absolute ethyl ether, and carrying out vacuum drying to obtain epoxy organosilicon quaternary ammonium salt, wherein the N, N-diethyl amine propyl methyl dimethoxy silane and the epoxy chloropropane react according to a molar ratio of 1:1;
step 3:
Mixing 35g of isophorone diisocyanate and 100g of polyethylene glycol 1000, reacting for 1h at 50 ℃ by taking dibutyl tin dilaurate as a catalyst, then adding 6.4g of dimethylolpropionic acid for reacting for 0.5h, and then adding 5.9g of 1, 4-butanediol for reacting for 1h to obtain an isocyanate group-terminated polyurethane prepolymer;
Step 4:
mixing 100g of epoxy polyurethane emulsion, 8g of epoxy flame retardant, 14g of epoxy organosilicon quaternary ammonium salt and 22g of curing agent to obtain a modifier, washing and drying polyester yarns, immersing the polyester yarns in the modifier for 60min according to a bath ratio of 1:20, taking out the polyester yarns, and vacuum-drying the polyester yarns at 80 ℃ for 3h to obtain modified polyester yarns;
step 5:
Dissolving carboxymethyl cellulose powder in deionized water to obtain carboxymethyl cellulose solution with the mass concentration of 10%, dissolving chitosan powder in acetic acid solution with the volume concentration of 3% to obtain chitosan solution with the mass concentration of 3%, mixing PVA solution and chitosan solution according to the volume ratio of 5:1, adding glycerol with the total mass of 3% of the mixed solution, mixing in an oil bath at 110 ℃ to obtain spinning solution, carrying out electrostatic spinning on the spinning solution to obtain bio-based spinning fibers, and blending 15% of bio-based spinning fibers and 85% of modified polyester yarns according to the weight percentage to obtain a finished product.
Example 2 an environment-friendly breathable polyester yarn fabric and a preparation process thereof, comprising the following steps:
Step 1:
S11, dispersing eugenol in ethyl acetate, cooling in an ice bath until the system temperature is stable by taking triethylamine as an acid binding agent, adding phenyl dichlorophosphate, stirring for 24 hours at 25 ℃, and finally separating, washing and rotary steaming the product to obtain phenyl di-eugenol phosphate, wherein eugenol and phenyl dichlorophosphate react according to a molar ratio of 2:1;
S12, dispersing phenyl diglucoside into ethyl acetate, stirring at 45 ℃ and adding m-chloroperoxybenzoic acid for reaction for 50 hours, separating liquid, washing, rotary steaming, cooling and recrystallizing a reaction product after the reaction is finished, and drying to obtain an epoxy flame retardant, wherein the phenyl diglucoside and the m-chloroperoxybenzoic acid react according to a molar ratio of 1:2;
step 2:
dispersing N, N-diethyl amine propyl methyl dimethoxy silane in absolute methanol under the nitrogen environment, heating to 60 ℃, adding a mixed solution of epoxy chloropropane and absolute methanol, after the addition is finished, carrying out heat preservation reaction for 8 hours, removing the absolute methanol by rotary evaporation, eluting with absolute ethyl ether, and carrying out vacuum drying to obtain epoxy organosilicon quaternary ammonium salt, wherein the N, N-diethyl amine propyl methyl dimethoxy silane and the epoxy chloropropane react according to a molar ratio of 1:1;
step 3:
Mixing 35g of isophorone diisocyanate and 100g of polyethylene glycol 1000, reacting for 1.5 hours at 55 ℃ by taking dibutyl tin dilaurate as a catalyst, then adding 6.4g of dimethylolpropionic acid for reacting for 1 hour, and then adding 5.9g of 1, 4-butanediol for reacting for 1.5 hours to obtain an isocyanate group-terminated polyurethane prepolymer;
Step 4:
Mixing 100g of epoxy polyurethane emulsion, 8g of epoxy flame retardant, 14g of epoxy organosilicon quaternary ammonium salt and 22g of curing agent to obtain a modifier, washing and drying polyester yarns, immersing the polyester yarns in the modifier for 75min according to a bath ratio of 1:20, taking out the polyester yarns, and vacuum-drying the polyester yarns at 85 ℃ for 4h to obtain modified polyester yarns;
step 5:
Dissolving carboxymethyl cellulose powder in deionized water to obtain carboxymethyl cellulose solution with the mass concentration of 10%, dissolving chitosan powder in acetic acid solution with the volume concentration of 3% to obtain chitosan solution with the mass concentration of 3%, mixing PVA solution and chitosan solution according to the volume ratio of 5:1, adding glycerol with the total mass of 3% of the mixed solution, mixing in an oil bath at 115 ℃ to obtain spinning solution, carrying out electrostatic spinning on the spinning solution to obtain bio-based spinning fibers, and blending 18% of bio-based spinning fibers and 82% of modified polyester yarns according to the weight percentage to obtain a finished product.
Example 3 an environment-friendly breathable polyester yarn fabric and a preparation process thereof, comprising the following steps:
Step 1:
s11, dispersing eugenol in ethyl acetate, cooling in an ice bath until the system temperature is stable by taking triethylamine as an acid binding agent, adding phenyl dichlorophosphate, stirring for 24 hours at 30 ℃, and finally separating, washing and rotary steaming the product to obtain phenyl di-eugenol phosphate, wherein eugenol and phenyl dichlorophosphate react according to a molar ratio of 2:1;
S12, dispersing phenyl diglucoside into ethyl acetate, stirring and adding m-chloroperoxybenzoic acid at 50 ℃ for reacting for 52 hours, and after the reaction is finished, separating liquid, washing, rotary steaming, cooling and recrystallizing the reaction product, and drying to obtain an epoxy flame retardant, wherein the phenyl diglucoside and the m-chloroperoxybenzoic acid react according to a molar ratio of 1:2;
step 2:
Dispersing N, N-diethyl amine propyl methyl dimethoxy silane in absolute methanol under the nitrogen environment, heating to 65 ℃, adding a mixed solution of epoxy chloropropane and absolute methanol, after the addition is finished, carrying out heat preservation reaction for 10 hours, removing the absolute methanol by rotary evaporation, eluting with absolute ethyl ether, and carrying out vacuum drying to obtain epoxy organosilicon quaternary ammonium salt, wherein the N, N-diethyl amine propyl methyl dimethoxy silane and the epoxy chloropropane react according to a molar ratio of 1:1;
step 3:
Mixing 35g of isophorone diisocyanate and 100g of polyethylene glycol 1000, reacting for 2 hours at 60 ℃ by taking dibutyltin dilaurate as a catalyst, then adding 6.4g of dimethylolpropionic acid for reacting for 1 hour, and then adding 5.9g of 1, 4-butanediol for reacting for 2 hours to obtain an isocyanate group-terminated polyurethane prepolymer;
Step 4:
Mixing 100g of epoxy polyurethane emulsion, 8g of epoxy flame retardant, 14g of epoxy organosilicon quaternary ammonium salt and 22g of curing agent to obtain a modifier, washing and drying polyester filaments, immersing the polyester filaments in the modifier for 90min according to a bath ratio of 1:20, taking out the polyester filaments, and vacuum-drying the polyester filaments at 90 ℃ for 5h to obtain modified polyester filaments;
step 5:
Dissolving carboxymethyl cellulose powder in deionized water to obtain carboxymethyl cellulose solution with the mass concentration of 10%, dissolving chitosan powder in acetic acid solution with the volume concentration of 3% to obtain chitosan solution with the mass concentration of 3%, mixing PVA solution and chitosan solution according to the volume ratio of 5:1, adding glycerol with the total mass of 3% of the mixed solution, mixing in an oil bath at 120 ℃ to obtain spinning solution, carrying out electrostatic spinning on the spinning solution to obtain bio-based spinning fibers, and blending 20% of bio-based spinning fibers and 85% of modified polyester yarns according to the weight percentage to obtain a finished product.
Comparative example 1 the polyester yarn was not modified and the remaining parameters were the same as in example 1.
Dissolving carboxymethyl cellulose powder in deionized water to obtain carboxymethyl cellulose solution with the mass concentration of 10%, dissolving chitosan powder in acetic acid solution with the volume concentration of 3% to obtain chitosan solution with the mass fraction of 3%, mixing PVA solution and chitosan solution according to the volume ratio of 5:1, adding glycerol with the total mass of 3% of the mixed solution, mixing in an oil bath at 110 ℃ to obtain spinning solution, carrying out electrostatic spinning on the spinning solution to obtain bio-based spinning fibers, and blending 15% of bio-based spinning fibers and 85% of polyester yarns according to the weight percentage to obtain a finished product.
Comparative example 2 without the addition of biobased spun fibers, the remaining parameters were the same as in example 2.
Step 1:
S11, dispersing eugenol in ethyl acetate, cooling in an ice bath until the system temperature is stable by taking triethylamine as an acid binding agent, adding phenyl dichlorophosphate, stirring for 24 hours at 25 ℃, and finally separating, washing and rotary steaming the product to obtain phenyl di-eugenol phosphate, wherein eugenol and phenyl dichlorophosphate react according to a molar ratio of 2:1;
S12, dispersing phenyl diglucoside into ethyl acetate, stirring at 45 ℃ and adding m-chloroperoxybenzoic acid for reaction for 50 hours, separating liquid, washing, rotary steaming, cooling and recrystallizing a reaction product after the reaction is finished, and drying to obtain an epoxy flame retardant, wherein the phenyl diglucoside and the m-chloroperoxybenzoic acid react according to a molar ratio of 1:2;
step 2:
dispersing N, N-diethyl amine propyl methyl dimethoxy silane in absolute methanol under the nitrogen environment, heating to 60 ℃, adding a mixed solution of epoxy chloropropane and absolute methanol, after the addition is finished, carrying out heat preservation reaction for 8 hours, removing the absolute methanol by rotary evaporation, eluting with absolute ethyl ether, and carrying out vacuum drying to obtain epoxy organosilicon quaternary ammonium salt, wherein the N, N-diethyl amine propyl methyl dimethoxy silane and the epoxy chloropropane react according to a molar ratio of 1:1;
step 3:
Mixing 35g of isophorone diisocyanate and 100g of polyethylene glycol 1000, reacting for 1.5 hours at 55 ℃ by taking dibutyl tin dilaurate as a catalyst, then adding 6.4g of dimethylolpropionic acid for reacting for 1 hour, and then adding 5.9g of 1, 4-butanediol for reacting for 1.5 hours to obtain an isocyanate group-terminated polyurethane prepolymer;
Step 4:
Mixing 100g of epoxy polyurethane emulsion, 8g of epoxy flame retardant, 14g of epoxy organosilicon quaternary ammonium salt and 22g of curing agent to obtain a modifier, washing and drying polyester fibers, immersing the polyester fibers in the modifier for 75min according to a bath ratio of 1:20, taking out the polyester fibers, and vacuum-drying the polyester fibers at 85 ℃ for 4h to obtain modified polyester fibers, and spinning the modified polyester fibers to obtain finished products.
Comparative example 3 the content of biobased spun fiber was increased and the remaining parameters were the same as in example 3.
Step 1:
s11, dispersing eugenol in ethyl acetate, cooling in an ice bath until the system temperature is stable by taking triethylamine as an acid binding agent, adding phenyl dichlorophosphate, stirring for 24 hours at 30 ℃, and finally separating, washing and rotary steaming the product to obtain phenyl di-eugenol phosphate, wherein eugenol and phenyl dichlorophosphate react according to a molar ratio of 2:1;
S12, dispersing phenyl diglucoside into ethyl acetate, stirring and adding m-chloroperoxybenzoic acid at 50 ℃ for reacting for 52 hours, and after the reaction is finished, separating liquid, washing, rotary steaming, cooling and recrystallizing the reaction product, and drying to obtain an epoxy flame retardant, wherein the phenyl diglucoside and the m-chloroperoxybenzoic acid react according to a molar ratio of 1:2;
step 2:
Dispersing N, N-diethyl amine propyl methyl dimethoxy silane in absolute methanol under the nitrogen environment, heating to 65 ℃, adding a mixed solution of epoxy chloropropane and absolute methanol, after the addition is finished, carrying out heat preservation reaction for 10 hours, removing the absolute methanol by rotary evaporation, eluting with absolute ethyl ether, and carrying out vacuum drying to obtain epoxy organosilicon quaternary ammonium salt, wherein the N, N-diethyl amine propyl methyl dimethoxy silane and the epoxy chloropropane react according to a molar ratio of 1:1;
step 3:
Mixing 35g of isophorone diisocyanate and 100g of polyethylene glycol 1000, reacting for 2 hours at 60 ℃ by taking dibutyltin dilaurate as a catalyst, then adding 6.4g of dimethylolpropionic acid for reacting for 1 hour, and then adding 5.9g of 1, 4-butanediol for reacting for 2 hours to obtain an isocyanate group-terminated polyurethane prepolymer;
Step 4:
Mixing 100g of epoxy polyurethane emulsion, 8g of epoxy flame retardant, 14g of epoxy organosilicon quaternary ammonium salt and 22g of curing agent to obtain a modifier, washing and drying polyester filaments, immersing the polyester filaments in the modifier for 90min according to a bath ratio of 1:20, taking out the polyester filaments, and vacuum-drying the polyester filaments at 90 ℃ for 5h to obtain modified polyester filaments;
step 5:
Dissolving carboxymethyl cellulose powder in deionized water to obtain carboxymethyl cellulose solution with the mass concentration of 10%, dissolving chitosan powder in acetic acid solution with the volume concentration of 3% to obtain chitosan solution with the mass fraction of 3%, mixing PVA solution and chitosan solution according to the volume ratio of 5:1, adding glycerol with the total mass of 3% of the mixed solution, mixing in an oil bath at 120 ℃ to obtain spinning solution, carrying out electrostatic spinning on the spinning solution to obtain bio-based spinning fibers, and blending 30% of bio-based spinning fibers and 70% of modified polyester yarns according to the weight percentage to obtain a finished product.
Experiment the performance test was performed on the finished products prepared in examples 1-3 and comparative examples 1-3.
Flame retardant property by cutting fabric into strip-shaped samples with the length of 10cm and the width of 1cm and testing the flame retardant property by adopting limiting oxygen index.
Air permeability performance air permeability was tested with reference to GB/T24218.15-2018, the average air flow through the samples was tested 3 times per sample using a fully automatic fabric air permeability tester, and the results were averaged.
Antibacterial performance, namely performing antibacterial test by referring to GB/T20944.2-2007, calculating antibacterial effect on escherichia coli by a plate counting method, and calculating a formula of antibacterial rate:
A=(C0-C)/C0×100%;
Wherein A is the antibacterial rate,% C 0 is the initial bacterial number, and C is the bacterial number (number) after antibacterial.
Anti-wrinkle elasticity the acute recovery angle of wrinkles was measured with reference to GB/T3819-1997 textile fabrics-test for recovery angle of fold test specimen.
The experimental results are shown in table 1.
TABLE 1 environmental protection breathable polyester filament fabric various performance test results
Project Limiting oxygen index Ventilation (mm/s) Antibacterial property Acute return angle of crease
Example 1 27.2% 897.5 99.4% 287°
Example 2 27.3% 914.8 99.5% 275°
Example 3 27.4% 925.1 99.5% 264°
Comparative example 1 19.6% 898.9 87.4% 290°
Comparative example 2 25.7% 723.6 99.5% 300°
Comparative example 3 27.6% 985.4 99.5% 229°
Conclusion the data of examples 1-3 show that the polyester yarn fabric prepared by the invention has excellent performance. The data of the example 1 and the comparative example 1 show that the flame retardant property and the antibacterial property of the fabric are obviously improved after the polyester yarn is modified by the modifier, the data of the example 2 and the comparative example 2 show that the addition of the bio-based spinning fiber is beneficial to improving the flame retardant property and the air permeability of the fabric, and the data of the example 3 and the comparative example 3 show that the excessive use amount of the bio-based spinning fiber can lead to the reduction of the crease resistance and the deterioration of the rebound resilience of the fabric.
It should be noted that the above-mentioned embodiments are merely preferred embodiments of the present invention, and the present invention is not limited thereto, but may be modified or substituted for some of the technical features thereof by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1.一种环保透气型涤丝面料的制备工艺,其特征在于:包括以下步骤:1. A process for preparing an environmentally friendly breathable polyester fabric, characterized in that it comprises the following steps: 步骤1:Step 1: 将环氧基聚氨酯乳液、环氧基阻燃剂、环氧基有机硅季铵盐、固化剂混合,得到改性剂;将涤丝洗涤干燥后,按浴比1:(15~20)浸渍于改性剂中60~90min,取出后在80~90℃下真空干燥3~5h,得到改性涤丝;The epoxy polyurethane emulsion, epoxy flame retardant, epoxy organosilicon quaternary ammonium salt and curing agent are mixed to obtain a modifier; after washing and drying the polyester yarn, the polyester yarn is immersed in the modifier at a bath ratio of 1:(15-20) for 60-90 minutes, and after taking out, the polyester yarn is vacuum dried at 80-90° C. for 3-5 hours to obtain a modified polyester yarn; 步骤2:Step 2: 将羧甲基纤维素粉末溶解于去离子水中得到质量浓度为10~15%的羧甲基纤维素溶液;将壳聚糖粉末溶于体积浓度为2~3%的乙酸溶液中,得到质量分数为2~3%的壳聚糖溶液;按体积比(3~5):1向羧甲基纤维素溶液种加入壳聚糖溶液,得到混合溶液;向混合溶液中加入混合溶液总质量1~3%的甘油,在110~120℃下油浴混合得到纺丝液;对纺丝液进行静电纺丝,得到生物基纺丝纤维;将生物基纺丝纤维、改性涤丝混纺,得到成品。The carboxymethyl cellulose powder is dissolved in deionized water to obtain a carboxymethyl cellulose solution with a mass concentration of 10-15%; the chitosan powder is dissolved in an acetic acid solution with a volume concentration of 2-3% to obtain a chitosan solution with a mass fraction of 2-3%; the chitosan solution is added to the carboxymethyl cellulose solution at a volume ratio of (3-5):1 to obtain a mixed solution; 1-3% of glycerol in the total mass of the mixed solution is added to the mixed solution, and the mixture is mixed in an oil bath at 110-120° C. to obtain a spinning solution; the spinning solution is subjected to electrostatic spinning to obtain a bio-based spinning fiber; and the bio-based spinning fiber and a modified polyester fiber are blended to obtain a finished product. 2.根据权利要求1所述的一种环保透气型涤丝面料的制备工艺,其特征在于:改性剂中,各组分含量,按重量份数计,100份环氧基聚氨酯乳液、5~8份环氧基阻燃剂、10~14份环氧基有机硅季铵盐、20~24份固化剂。2. The preparation process of an environmentally friendly breathable polyester fabric according to claim 1 is characterized in that: the content of each component in the modifier, by weight, is 100 parts of epoxy polyurethane emulsion, 5 to 8 parts of epoxy flame retardant, 10 to 14 parts of epoxy silicone quaternary ammonium salt, and 20 to 24 parts of curing agent. 3.根据权利要求1所述的一种环保透气型涤丝面料的制备工艺,其特征在于:环氧基聚氨酯乳液的制备方法为:按重量份数计,取35~50份异佛尔酮二异氰酸酯、100份聚乙二醇1000混合,以二月桂酸二丁基锡为催化剂,在50~60℃下反应1~2h,然后加入6~8份二羟甲基丙酸反应0.5~1h,再加5~7份1,4-丁二醇反应1~2h,得到异氰酸酯基封端聚氨酯预聚体;按异氰酸酯基与羟基摩尔比1:1加入缩水甘油反应1~2h,冷却加入9~13份三乙胺中和反应,加入去离子水乳化得到固含量为30~40%环氧基聚氨酯乳液。3. The preparation process of an environmentally friendly breathable polyester fabric according to claim 1 is characterized in that: the preparation method of the epoxy polyurethane emulsion is as follows: by weight, 35 to 50 parts of isophorone diisocyanate and 100 parts of polyethylene glycol 1000 are mixed, dibutyltin dilaurate is used as a catalyst, and the mixture is reacted at 50 to 60° C. for 1 to 2 hours, and then 6 to 8 parts of dihydroxymethylpropionic acid are added to react for 0.5 to 1 hour, and then 5 to 7 parts of 1,4-butanediol are added to react for 1 to 2 hours to obtain an isocyanate-terminated polyurethane prepolymer; glycidol is added at a molar ratio of isocyanate group to hydroxyl group of 1:1 to react for 1 to 2 hours, cooled, 9 to 13 parts of triethylamine are added for neutralization reaction, and deionized water is added for emulsification to obtain an epoxy polyurethane emulsion with a solid content of 30 to 40%. 4.根据权利要求1所述的一种环保透气型涤丝面料的制备工艺,其特征在于:环氧基阻燃剂的制备方法,包括以下步骤:4. The process for preparing an environmentally friendly breathable polyester fabric according to claim 1, characterized in that: the preparation method of the epoxy flame retardant comprises the following steps: S1:将丁香酚分散在乙酸乙酯中,以三乙胺作为缚酸剂,冰浴中冷却至体系温度稳定后,加入二氯化磷酸苯酯,在20~30℃下搅拌24h,最后将产物进行分液、洗涤和旋蒸得到二丁香酚基磷酸苯酯;S1: Disperse eugenol in ethyl acetate, use triethylamine as an acid-binding agent, cool in an ice bath until the system temperature is stable, add phenyl dichlorophosphate, stir at 20-30°C for 24h, and finally separate, wash and rotary evaporate the product to obtain dieugenol phenyl phosphate; S2:将二丁香酚基磷酸苯酯分散在乙酸乙酯中,在40~50℃下搅拌加入间氯过氧苯甲酸反应48~52h;反应结束后对反应产物进行分液、洗涤、旋蒸、降温重结晶,干燥得到环氧基阻燃剂。S2: Disperse dieugenol phenyl phosphate in ethyl acetate, add m-chloroperbenzoic acid at 40-50° C. with stirring and react for 48-52 hours; after the reaction, separate the reaction product, wash, rotary evaporate, cool and recrystallize, and dry to obtain an epoxy flame retardant. 5.根据权利要求4所述的一种环保透气型涤丝面料的制备工艺,其特征在于:S1中,丁香酚与二氯化磷酸苯酯按摩尔比2:1进行反应。5. The process for preparing an environmentally friendly breathable polyester fabric according to claim 4, characterized in that: in S1, eugenol and phenyl dichloride phosphate are reacted in a molar ratio of 2:1. 6.根据权利要求4所述的一种环保透气型涤丝面料的制备工艺,其特征在于:S2中,二丁香酚基磷酸苯酯与间氯过氧苯甲酸按摩尔比1:2进行反应。6. The process for preparing an environmentally friendly breathable polyester fabric according to claim 4, characterized in that: in S2, dieugenol phenyl phosphate and meta-chloroperbenzoic acid react in a molar ratio of 1:2. 7.根据权利要求1所述的一种环保透气型涤丝面料的制备工艺,其特征在于:环氧基有机硅季铵盐的制备方法为:在氮气环境下,将N,N-二乙基胺丙基甲基二甲氧基硅烷分散在和无水甲醇中,升温至55~65℃,加入环氧氯丙烷和无水甲醇的混合溶液,保温反应6~10h,旋蒸除去无水甲醇并用无水乙醚洗脱,真空干燥得到环氧基有机硅季铵盐。7. The preparation process of an environmentally friendly breathable polyester fabric according to claim 1 is characterized in that: the preparation method of epoxy silicone quaternary ammonium salt is: in a nitrogen environment, N, N-diethylaminopropylmethyldimethoxysilane is dispersed in anhydrous methanol, the temperature is raised to 55-65°C, a mixed solution of epichlorohydrin and anhydrous methanol is added, the temperature is kept for 6-10 hours, the anhydrous methanol is removed by rotary evaporation and eluted with anhydrous ether, and the epoxy silicone quaternary ammonium salt is obtained by vacuum drying. 8.根据权利要求7所述的一种环保透气型涤丝面料的制备工艺,其特征在于:N,N-二乙基胺丙基甲基二甲氧基硅烷与环氧氯丙烷按摩尔比1:1进行反应。8. A process for preparing an environmentally friendly breathable polyester fabric according to claim 7, characterized in that: N,N-diethylaminopropylmethyldimethoxysilane and epichlorohydrin are reacted in a molar ratio of 1:1. 9.根据权利要求1所述的一种环保透气型涤丝面料的制备工艺,其特征在于:环保透气型涤丝面料中,按重量百分数计,15~20%生物基纺丝纤维、80~85%改性涤丝混纺。9. The process for preparing an environmentally friendly breathable polyester fabric according to claim 1, characterized in that the environmentally friendly breathable polyester fabric contains, by weight percentage, 15-20% bio-based spinning fibers and 80-85% modified polyester blended fibers. 10.根据权利要求1~9中任一项所述的制备工艺制备得到的环保透气型涤丝面料。10. The environmentally friendly breathable polyester fabric prepared by the preparation process according to any one of claims 1 to 9.
CN202411658422.8A 2024-11-20 2024-11-20 Environmentally friendly breathable polyester fabric and preparation process thereof Pending CN119392504A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN119571624A (en) * 2025-02-08 2025-03-07 比音勒芬服饰股份有限公司 A windproof and breathable composite fabric and its application
CN119978753A (en) * 2025-04-15 2025-05-13 安徽正杰科技有限公司 A kind of conductive unsaturated polyester resin and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN119571624A (en) * 2025-02-08 2025-03-07 比音勒芬服饰股份有限公司 A windproof and breathable composite fabric and its application
CN119978753A (en) * 2025-04-15 2025-05-13 安徽正杰科技有限公司 A kind of conductive unsaturated polyester resin and preparation method thereof

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