A cooling high-elastic fiber, its preparation method and application

By using a method to prepare cool-feeling high-elastic fibers and utilizing a core-shell structure modifier to enhance coolness and elasticity, the problem of loss of elasticity and reduced coolness in cool-feeling high-elastic polyester fibers after long-term use has been solved, thus achieving efficient maintenance of the fiber's coolness and high elasticity.

CN120866969BActive Publication Date: 2026-03-06SHANTOU CANXINSHENG TEXTILE TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202511234342.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-09-01
Publication Date
2026-03-06
Estimated Expiration
2045-09-01

AI Technical Summary

Technical Problem

Existing cool-feeling high-elastic polyester fibers are prone to loss of elasticity and reduced coolness after long-term use.

Method used

Cooling-feeling polyester POY precursor yarn is blended with a modifier and melt-spun, and then processed through a texturing process to prepare a cooling-feeling high-elastic fiber. The modifier consists of rare earth-doped yttrium zirconate as the core and hexagonal boron nitride nanosheets as the shell, forming a core-shell structure. The cooling sensation and elasticity are synergistically enhanced by the core's reflection of near-infrared thermal radiation and the shell's thermal conductivity.

Benefits of technology

It significantly improves the cooling properties, elastic recovery rate, durability, and washability of fibers, maintaining the cooling and elasticity of fibers even after multiple washes.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention discloses a cooling-feeling high-elastic fiber, its preparation method, and its application, relating to the field of high-performance fiber technology. The invention discloses a method for preparing a cooling-feeling high-elastic fiber, comprising the following steps: melt-blending and extruding a modifier, an antioxidant, and polyester chips to obtain a cooling-feeling masterbatch; melt-spinning the cooling-feeling masterbatch and polyester chips to obtain a cooling-feeling polyester POY precursor yarn; and performing a texturing process on the cooling-feeling polyester POY precursor yarn to obtain a cooling-feeling high-elastic fiber. The cooling-feeling high-elastic fiber prepared in this application is then spun to obtain a cooling-feeling high-elastic fabric, which retains high elasticity and cooling properties even after multiple washes.
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Description

Technical Field

[0001] This invention relates to the field of high-performance fiber technology, specifically to a cool-feeling high-elastic fiber, its preparation method, and its application. Background Technology

[0002] Elastic fibers are fibers with high elongation at break, low modulus, and high elastic recovery, with spandex being the most representative variety. Currently, spandex is widely used in textiles, knitted products with elastic properties, and in the production of medical elastic bandages. Due to the relatively complex production process of spandex, its processing costs are higher and environmental requirements are stricter compared to melt-spun fibers. Therefore, for many years, the chemical fiber industry has focused on researching and developing polyester elastic fibers to easily replace the expensive spandex. However, polyester fibers also have many disadvantages, such as poor moisture absorption, a tendency to generate static electricity, and a stuffy feeling when worn.

[0003] Currently, the manufacturing of cooling textiles mainly employs two technologies: the first is to reduce the thermal resistance of the textile and increase its thermal conductivity, allowing the heat generated by the human body to be released and dissipated rapidly; the second is to utilize phase change materials, which use the principle of heat release and absorption during solid-liquid phase changes to absorb the heat generated by the human body, making the body feel cool and comfortable. However, with increased wear time and washing cycles, these fabrics tend to lose elasticity and experience a decrease in cooling performance, affecting the fabric's shape and functional properties. Summary of the Invention

[0004] The purpose of this invention is to provide a cool-feeling high-elastic fiber and its preparation method, and to solve the following technical problems: existing cool-feeling high-elastic polyester fibers are prone to loss of elasticity and reduced coolness after long-term use.

[0005] The objective of this invention can be achieved through the following technical solution: a method for preparing a cool-feeling high-elastic fiber, comprising the following steps: subjecting cool-feeling polyester POY precursor yarn to a texturing process to obtain cool-feeling high-elastic fiber; the cool-feeling polyester POY precursor yarn is obtained by melt spinning a blend of cool-feeling masterbatch and polyester chips;

[0006] The cooling masterbatch is obtained by melt blending a modifier, an antioxidant, and polyester chips; the preparation method of the modifier includes the following steps:

[0007] S1: Add erbium nitrate and deionized water to reactor A for dispersion, add urea to adjust pH to 3-6, control temperature at 120-150℃ and keep the reaction at this temperature for 6-12 hours, centrifuge, wash, dry, sinter, and grind to obtain nanoparticles;

[0008] S2: Epoxy-modified hexagonal boron nitride powder, N,N-dimethylformamide, and nanoparticles are added to reactor B and dispersed. The temperature is controlled at 25-35℃ and the reaction is maintained at this temperature for 8-12 hours. After centrifugation, washing, and drying, core-shell particles are obtained.

[0009] S3: In a nitrogen atmosphere, core-shell particles, N,N-dimethylformamide, 4-carboxy-benzenesulfonyl azide, and triphenylphosphine are added to reactor C. The temperature is controlled at 100-110℃ and the reaction is carried out under stirring for 12-24 hours. The mixture is then centrifuged, washed, dried, and ground to obtain the modifier.

[0010] As a further aspect of the present invention, the texturing process includes the following steps:

[0011] A1: Pull the cooling polyester POY raw yarn into the pre-network nozzle for pre-networking treatment;

[0012] A2: The pre-networked filaments are sequentially passed through the guide and the first roller to the first heating box for heating, plasticizing, stretching and deformation;

[0013] A3: The stretched and deformed filaments are then false-twisted by the false twister;

[0014] A4: The false-twisted yarn is drawn into the main network nozzle through the second roller for network processing;

[0015] A5: The processed wires enter the second heating box for heat setting;

[0016] A6: After heat setting, the filaments enter the third roller for stretching, are oiled by the oiling roller, and finally wound by the winding roller to obtain cool-feeling high-elastic fiber.

[0017] As a further aspect of the present invention: the processing pressure of the pre-network nozzle is 0.04-0.05 MPa, the processing pressure of the main network nozzle is 0.12-0.16 MPa; the deformation temperature of the first hot box is 195-200℃, the shaping temperature of the second hot box is 85-95℃; the D / Y ratio of the false twister is 1.65-1.85; the second roller speed is 700m / min-800m / min, the stretching ratio is 1.7-1.75; the shaping overfeed rate is 4.9-5.4, and the winding overfeed rate is 4.1-4.3.

[0018] As a further aspect of the present invention: the mass ratio of cooling masterbatch to polyester chips in the cooling polyester POY precursor yarn is 1-10:100; the masterbatch contains the following raw materials by weight percentage: 0.5-10% modifier, 0.1-1% antioxidant, and the balance being polyester chips, the sum of which is 100% by weight; the antioxidant is one or more of hindered phenolic antioxidants, triazole antioxidants, phosphite antioxidants, and thioester antioxidants, mixed in any proportion.

[0019] As a further embodiment of the present invention, the preparation method of epoxy-modified hexagonal boron nitride powder includes the following steps: adding h-BN powder, concentrated ammonia, and isopropanone into a reaction flask, controlling the temperature at 0-5℃, treating under stirring conditions for 6-9 hours, centrifuging, taking the supernatant and adjusting the pH of the supernatant to 4-5, adding (3-glycidyl etheroxypropyl)trimethoxysilane, controlling the temperature at 50-60℃, reacting under stirring conditions for 12-24 hours, filtering, washing, and drying to obtain epoxy-modified hexagonal boron nitride powder.

[0020] As a further embodiment of the present invention: the addition ratio of h-BN powder, concentrated ammonia, isopropyl ketone, and (3-glycidyl etheroxypropyl)trimethoxysilane is 5-10g: 200-400mL: 100-500mL: 10-20mL.

[0021] As a further aspect of the present invention: the addition ratio of yttrium nitrate, zirconium nitrate, erbium nitrate and deionized water in S1 is 23.5-24g: 10g: 0.45-0.8g: 500-1000mL.

[0022] As a further aspect of the present invention: the addition ratio of yttrium nitrate, zirconium nitrate, erbium nitrate and deionized water in S1 is 23.5-24g: 10g: 0.45-0.8g: 500-1000mL.

[0023] As a further aspect of the present invention: drying specifically involves heating to 250-350℃ and processing for 10-20 minutes; sintering specifically involves annealing at 800-900℃ in a muffle furnace for 2-4 hours.

[0024] As a further embodiment of the present invention: the addition ratio of epoxy-modified hexagonal boron nitride powder, N,N-dimethylformamide, and nanoparticles in S2 is 10-20g: 200-400mL: 10g.

[0025] As a further embodiment of the present invention: the addition ratio of core-shell particles, N,N-dimethylformamide, 4-carboxy-benzenesulfonyl azide, and triphenylphosphine in S3 is 10g: 200-400mL: 10-15g: 0.1-1g.

[0026] A cool-feeling high-elastic fiber, made by any of the above preparation methods.

[0027] The aforementioned cool-feeling high-elastic fibers are used in fabrics.

[0028] The beneficial effects of this invention are:

[0029] (1) Constructing a core-shell structure to impart cooling properties to the material

[0030] This application describes a modifier prepared using rare-earth-doped yttrium zirconate as the core, functionalized hexagonal boron nitride nanosheets as the shell encapsulating and connecting the core, and 4-carboxy-benzenesulfonyl azide as a bridge. The core is composed of rare-earth Er... 3+ Yttrium zirconate-doped nanoparticles exhibit extremely high reflectivity to near-infrared thermal radiation emitted by the human body, reflecting heat back instead of being absorbed by the skin or fabric, thus producing a significant and sustained cooling sensation. Hexagonal boron nitride nanosheets, as an extremely stable ceramic material, possess excellent high-temperature resistance and chemical corrosion resistance, protecting the core from acidic environments during processing. The high thermal conductivity of hexagonal boron nitride nanosheets enhances the instantaneous cooling sensation and promotes more uniform crystallization during fiber cooling and heat treatment, facilitating the formation of a more regular crystal structure. The layered structure of the hexagonal boron nitride nanosheets effectively physically blocks polymer molecular chains, stabilizing crystal nuclei during heterogeneous nucleation and the coiled structure during subsequent fiber deformation, providing additional benefits for improving elastic recovery. The modifier prepared in this application utilizes the radiative cooling effect of the core and the conductive cooling effect of the shell to enhance the cooling performance of polyester fibers.

[0031] (2) It provides a high specific surface area and abundant nucleation sites, giving the material high resilience.

[0032] The modifier prepared in this application acts as a nucleating agent during the spinning and texturing process of cool-feeling polyester POY, exhibiting heterogeneous nucleation and grain refinement effects. The modifier induces polyester molecules to crystallize on its surface, forming more numerous and smaller crystals. This refined crystal structure serves as a physical crosslinking point, effectively fixing the macromolecular chain network in the amorphous region, allowing the fiber to recover better after deformation, significantly improving the fiber's elastic recovery rate and durability. The crosslinking of the modifier with the polyester molecular chains effectively hinders the slippage of macromolecular chains, not only resulting in a stable crimp structure formed during false twisting, reducing boiling water shrinkage and making the crimp more durable; but also giving it better plasticity in subsequent deformation, which is beneficial for forming a full crimp. The cool-feeling high-elastic fiber prepared in this application exhibits excellent crimp shrinkage rate, crimp stability, and elastic recovery rate.

[0033] (3) Crosslinking with polyester through chemical bonds, giving the fabric water-washing resistance.

[0034] The modifier prepared in this application has azide groups grafted onto its surface. At PET processing temperatures, these azide groups decompose and directly insert into the CH bonds of the PET molecular chain, forming strong covalent bonds. This application utilizes refined microcrystals to achieve physical crosslinking and chemical bonding to achieve molecular chain network crosslinking. The combined effect of these two methods makes the interfacial bond between the modified particles and the PET matrix less susceptible to erosion and damage. Under washing (especially high-temperature washing) and mechanical force, the possibility of the modifier detaching from the fiber surface or interior is reduced, maintaining the fiber's cooling properties; moreover, it improves the stability of the molecular chain network, allowing the fiber to quickly recover after deformation and achieving durable functionality. Detailed Implementation

[0035] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0036] Example 1

[0037] The preparation method of the modifier includes the following steps:

[0038] S1: 23.5g yttrium nitrate, 10g zirconium nitrate, 0.45g erbium nitrate, and 500mL deionized water were added to reactor A for dispersion. Urea was added to adjust the pH to 3. The temperature was controlled at 120℃ and the reaction was maintained at this temperature for 6 hours. The mixture was then centrifuged, washed, heated to 350℃ for 20 minutes, sintered in a muffle furnace at 900℃ for 2 hours, and ground to obtain nanoparticles.

[0039] S2: Add 5g h-BN powder, 200mL concentrated ammonia and 100mL isopropanone to a reaction flask, control the temperature at 0℃ and stir for 6h, centrifuge, take the supernatant and adjust the pH of the supernatant to 4, add 10mL (3-glycidyl ether oxypropyl)trimethoxysilane, control the temperature at 50℃ and stir for 12h, filter, wash and dry to obtain epoxy modified hexagonal boron nitride powder;

[0040] 5g of epoxy-modified hexagonal boron nitride powder, 100mL of N,N-dimethylformamide, and 5g of nanoparticles were added to reactor B and dispersed. The temperature was controlled at 25℃ and the reaction was kept at this temperature for 8h. After centrifugation, washing, and drying, core-shell particles were obtained.

[0041] S3: In a nitrogen atmosphere, 5g of core-shell particles, 100mL of N,N-dimethylformamide, 5g of 4-carboxy-benzenesulfonyl azide, and 0.05g of triphenylphosphine were added to reactor C. The reaction was carried out at 100℃ with stirring for 12h. The mixture was then centrifuged, washed, dried, and ground to obtain the modifier.

[0042] Example 2

[0043] The preparation method of the modifier includes the following steps:

[0044] S1: 23.5g of yttrium nitrate, 10g of zirconium nitrate, 0.7g of erbium nitrate, and 700mL of deionized water were added to reactor A for dispersion. Urea was added to adjust the pH to 4. The temperature was controlled at 135℃ and the reaction was maintained at this temperature for 9h. After centrifugation, washing, heating to 350℃ for 20min, sintering at 900℃ in a muffle furnace for 2h, and grinding, nanoparticles were obtained.

[0045] S2: Add 7g h-BN powder, 300mL concentrated ammonia, and 300mL isopropanone to a reaction flask. Control the temperature at 0℃ and treat under stirring for 9h. Centrifuge, collect the supernatant and adjust the pH of the supernatant to 5. Add 15mL (3-glycidyl ether oxypropyl)trimethoxysilane. Control the temperature at 55℃ and react under stirring for 18h. Filter, wash, and dry to obtain epoxy-modified hexagonal boron nitride powder. Add 7g epoxy-modified hexagonal boron nitride powder, 150mL N,N-dimethylformamide, and 5g nanoparticles to reaction vessel B and disperse. Control the temperature at 30℃ and keep the reaction at this temperature for 10h. Centrifuge, wash, and dry to obtain core-shell particles.

[0046] S3: In a nitrogen atmosphere, 5g of core-shell particles, 150mL of N,N-dimethylformamide, 6.5g of 4-carboxy-benzenesulfonyl azide, and 0.1g of triphenylphosphine were added to reactor C. The reaction was carried out at 100℃ with stirring for 18h. The mixture was then centrifuged, washed, dried, and ground to obtain the modifier.

[0047] Example 3

[0048] The preparation method of the modifier includes the following steps:

[0049] S1: 24g of yttrium nitrate, 10g of zirconium nitrate, 0.8g of erbium nitrate, and 1000mL of deionized water were added to reactor A for dispersion. Urea was added to adjust the pH to 6. The temperature was controlled at 150℃ and the reaction was maintained at this temperature for 12h. The mixture was then centrifuged, washed, heated to 350℃ for 20min, sintered in a muffle furnace at 900℃ for 2h, and ground to obtain nanoparticles.

[0050] S2: Add 10g h-BN powder, 400mL concentrated ammonia, and 500mL isopropanone to a reaction flask. Control the temperature at 5℃ and treat under stirring for 9h. Centrifuge, collect the supernatant and adjust the pH of the supernatant to 5. Add 20mL (3-glycidyl ether oxypropyl)trimethoxysilane. Control the temperature at 60℃ and react under stirring for 24h. Filter, wash, and dry to obtain epoxy-modified hexagonal boron nitride powder. Add 10g epoxy-modified hexagonal boron nitride powder, 200mL N,N-dimethylformamide, and 5g nanoparticles to reaction vessel B and disperse. Control the temperature at 35℃ and keep the reaction at this temperature for 12h. Centrifuge, wash, and dry to obtain core-shell particles.

[0051] S3: In a nitrogen atmosphere, 5g of core-shell particles, 200mL of N,N-dimethylformamide, 7.5g of 4-carboxy-benzenesulfonyl azide, and 0.5g of triphenylphosphine were added to reactor C. The reaction was carried out at 110℃ with stirring for 24h. The mixture was then centrifuged, washed, dried, and ground to obtain the modifier.

[0052] Example 4

[0053] A method for preparing a cooling, high-elastic fiber includes the following steps:

[0054] A1: Melt blending: 5g of the modifier prepared in Example 1, 0.5g of bis(2,6-di-tert-butyl-4-methylphenyl) pentaerythritol diphosphite, and 94.5g of polyester chips (purchased from Hubei Xinfeng Chemical Fiber Co., Ltd., intrinsic viscosity 0.68dL / g, end carboxyl group content 21.1mol / t) were melt blended to obtain a cooling masterbatch;

[0055] A2: Melt spinning: 10g of cooling masterbatch is blended with 100g of polyester chips (purchased from Hubei Xinfeng Chemical Fiber Co., Ltd., intrinsic viscosity 0.68dL / g, end carboxyl content 21.1mol / t) and melt spun (screw pressure 100kg / cm²). 2 The process involves: screw speed of 20 r / min, melt spinning temperature of 290℃, side blowing cooling (spinneret ring blowing, air temperature of 34℃, humidity of 55%, air speed of 0.4 m / s); oiling and bundling (oiling rate of 1.2%), and winding to obtain 140 dtex / 36f cool-feel polyester POY precursor yarn.

[0056] A3: Texturing Treatment: The cool-feeling polyester POY filament is drawn into the pre-network nozzle and processed at a pressure of 0.05 MPa for pre-network treatment; the pre-network treated filament is then passed through the guide and the first roller to the first hot box at a deformation temperature of 197℃ for heating, plasticizing, and stretching deformation; the stretched filament enters the false twister and is false twisted with a D / Y ratio controlled at 1.68; the false-twisted filament is then drawn into the main network nozzle through the second roller at a pressure of 0.13 MPa for network processing; the networked filament enters the second hot box at a setting temperature of 92℃ for heat setting; the heat-set filament enters the third roller for stretching, is oiled by the oiling roller, and finally wound by the winding roller to obtain cool-feeling high-elastic fiber.

[0057] The second roller speed is 700 m / min, the stretching ratio is 1.72, the setting overfeed rate is 5.1, and the winding overfeed rate is 4.2.

[0058] Example 5

[0059] A method for preparing a cool-feeling high-elastic fiber, which is the same as that in Example 4 except that the modifier prepared in Example 1 is replaced in equal amounts with the modifier prepared in Example 2, and the remaining components and preparation method are the same as in Example 4.

[0060] Example 6

[0061] A method for preparing a cool-feeling high-elastic fiber, which is the same as that in Example 4 except that the modifier prepared in Example 1 is replaced in equal amounts with the modifier prepared in Example 3, and the remaining components and preparation method are the same as in Example 4.

[0062] Comparative Example 1

[0063] The preparation method of the modifier includes the following steps:

[0064] S1: 23.5g of yttrium nitrate, 10g of zirconium nitrate, 0.7g of erbium nitrate, and 700mL of deionized water were added to reactor A for dispersion. Urea was added to adjust the pH to 4. The temperature was controlled at 135℃ and the reaction was maintained at this temperature for 9h. After centrifugation, washing, heating to 350℃ for 20min, sintering at 900℃ in a muffle furnace for 2h, and grinding, nanoparticles were obtained.

[0065] S2: Add 7g h-BN powder, 300mL concentrated ammonia, and 300mL isopropanone to a reaction flask. Control the temperature at 0℃ and treat under stirring for 9h. Centrifuge, take the supernatant and adjust the pH of the supernatant to 5. Add 15mL (3-glycidyl ether oxypropyl)trimethoxysilane. Control the temperature at 55℃ and react under stirring for 18h. Filter, wash, and dry to obtain epoxy-modified hexagonal boron nitride powder. Add 7g epoxy-modified hexagonal boron nitride powder, 150mL N,N-dimethylformamide, and 5g nanoparticles to reaction vessel B and disperse. Control the temperature at 30℃ and keep the reaction at this temperature for 10h. Centrifuge, wash, and dry to obtain the modifier.

[0066] Comparative Example 2

[0067] The preparation method of the modifier includes the following steps:

[0068] S1: 23.5g of yttrium nitrate, 10g of zirconium nitrate, and 700mL of deionized water were added to reactor A for dispersion. Urea was added to adjust the pH to 4. The temperature was controlled at 135℃ and the reaction was kept at this temperature for 9h. After centrifugation, washing, heating to 350℃ for 20min, sintering at 900℃ in a muffle furnace for 2h, and grinding, nanoparticles were obtained.

[0069] S2: Add 7g h-BN powder, 300mL concentrated ammonia, and 300mL isopropanone to a reaction flask. Control the temperature at 0℃ and treat under stirring for 9h. Centrifuge, collect the supernatant and adjust the pH of the supernatant to 5. Add 15mL (3-glycidyl ether oxypropyl)trimethoxysilane. Control the temperature at 55℃ and react under stirring for 18h. Filter, wash, and dry to obtain epoxy-modified hexagonal boron nitride powder. Add 7g epoxy-modified hexagonal boron nitride powder, 150mL N,N-dimethylformamide, and 5g nanoparticles to reaction vessel B and disperse. Control the temperature at 30℃ and keep the reaction at this temperature for 10h. Centrifuge, wash, and dry to obtain core-shell particles.

[0070] S3: In a nitrogen atmosphere, 5g of core-shell particles, 150mL of N,N-dimethylformamide, 6.5g of 4-carboxy-benzenesulfonyl azide, and 0.1g of triphenylphosphine were added to reactor C. The reaction was carried out at 100℃ with stirring for 18h. The mixture was then centrifuged, washed, dried, and ground to obtain the modifier.

[0071] Comparative Example 3

[0072] The preparation method of the modifier includes the following steps:

[0073] S1: 23.5g of yttrium nitrate, 10g of zirconium nitrate, 0.7g of erbium nitrate, and 700mL of deionized water were added to reactor A for dispersion. Urea was added to adjust the pH to 4. The temperature was controlled at 135℃ and the reaction was maintained at this temperature for 9h. After centrifugation, washing, heating to 350℃ for 20min, sintering at 900℃ in a muffle furnace for 2h, and grinding, nanoparticles were obtained.

[0074] S2: Add 7g of nanoparticles, 300mL of concentrated ammonia, and 300mL of isopropanone to a reaction flask. Control the temperature at 0℃ and stir for 9h. Centrifuge, take the supernatant and adjust the pH of the supernatant to 5. Add 15mL of (3-glycidyl etheroxypropyl)trimethoxysilane, control the temperature at 55℃ and stir for 18h. Filter, wash, and dry to obtain epoxy-modified nanoparticles.

[0075] S3: In a nitrogen atmosphere, 5g of epoxy-modified nanoparticles, 150mL of N,N-dimethylformamide, 6.5g of 4-carboxy-benzenesulfonyl azide, and 0.1g of triphenylphosphine were added to reactor C. The reaction was carried out at 100℃ with stirring for 18h. The mixture was then centrifuged, washed, dried, and ground to obtain the modifier.

[0076] Comparative Example 4

[0077] The preparation method of the modifier includes the following steps:

[0078] S1: 23.5g of yttrium nitrate, 10g of zirconium nitrate, 0.7g of erbium nitrate, and 700mL of deionized water were added to reactor A for dispersion. Urea was added to adjust the pH to 4. The temperature was controlled at 135℃ and the reaction was maintained at this temperature for 9h. After centrifugation, washing, heating to 350℃ for 20min, sintering at 900℃ in a muffle furnace for 2h, and grinding, nanoparticles were obtained.

[0079] S2: Add 7g of nanoparticles, 300mL of concentrated ammonia, and 300mL of isopropanone to a reaction flask. Control the temperature at 0℃ and treat under stirring for 9h. Centrifuge, collect the supernatant, and adjust the pH of the supernatant to 5. Add 15mL of (3-glycidyl ether oxypropyl)trimethoxysilane. Control the temperature at 55℃ and react under stirring for 18h. Filter, wash, and dry to obtain epoxy-modified nanoparticles. Add 7g of hexagonal boron nitride powder, 150mL of N,N-dimethylformamide, and 5g of epoxy-modified nanoparticles to reaction vessel B and disperse. Control the temperature at 30℃ and keep the reaction at this temperature for 10h. Centrifuge, wash, and dry to obtain core-shell particles.

[0080] S3: In a nitrogen atmosphere, 5g of core-shell particles, 150mL of N,N-dimethylformamide, 6.5g of 4-carboxy-benzenesulfonyl azide, and 0.1g of triphenylphosphine were added to reactor C. The reaction was carried out at 100℃ with stirring for 18h. The mixture was then centrifuged, washed, dried, and ground to obtain the modifier.

[0081] Comparative Example 5

[0082] A method for preparing a cool-feeling high-elastic fiber, which is the same as that in Example 4 except that the modifier prepared in Example 1 is replaced in equal amounts with the modifier prepared in Comparative Example 1, and the remaining components and preparation methods are the same as in Example 4.

[0083] Comparative Example 6

[0084] A method for preparing a cool-feeling high-elastic fiber, which is the same as that in Example 4 except that the modifier prepared in Example 1 is replaced in equal amounts with the modifier prepared in Comparative Example 2, and the remaining components and preparation method are the same as in Example 4.

[0085] Comparative Example 7

[0086] A method for preparing a cool-feeling high-elastic fiber, which is the same as that in Example 4 except that the modifier prepared in Example 1 is replaced in equal amounts with the modifier prepared in Comparative Example 3, and the remaining components and preparation method are the same as in Example 4.

[0087] Comparative Example 8

[0088] A method for preparing a cool-feeling high-elastic fiber, which is the same as that in Example 4 except that the modifier prepared in Example 1 is replaced in equal amounts with the modifier prepared in Comparative Example 4, and the remaining components and preparation method are the same as in Example 4.

[0089] Performance testing:

[0090] (1) Cooling performance

[0091] According to GB / T 35263-2017 "Test and Evaluation of Instant Cooling Properties of Textiles", the contact cooling sensation (Q-max value) of the materials was tested. The fibers prepared in Examples 4-6 and Comparative Examples 5-8 were washed 20 times according to the 4N program and hung to dry according to GB / T 8629-2017 "Home Washing and Drying Procedures for Textile Testing" and the Q-max value was tested again, and the cooling sensation retention rate was calculated. The test results are shown in Table 1.

[0092] Table 1: Statistical Table of Cooling Performance Test Data for Examples 4-6 and Comparative Examples 5-8

[0093]

[0094] As shown in Table 1, the experimental data indicate that the contact cooling coefficients of Examples 4-6 range from 0.26 to 0.29 W / cm². 2 The Q-max value of the embodiment was significantly higher than that of the comparative examples 5-8, demonstrating good contact cooling sensation. Even after 20 washes, the cooling sensation retention rate of the embodiment was high, while that of the comparative examples was less than 90%, indicating that the cooling sensation performance of the comparative examples was significantly reduced and the long-term cooling sensation performance was poor.

[0095] (2) Elastic recovery rate

[0096] a. Single tensile recovery performance: According to GB / T 3923.1-2013 "Textiles - Tensile properties of fabrics - Part 1: Determination of breaking strength and elongation at break (strip method)", the specimen is stretched to a fixed elongation of 5%, and then allowed to recover. The deformation that cannot recover (plastic deformation) and the deformation that can recover (elastic deformation) are measured.

[0097] Elastic recovery rate R(%) = (L1-L2) / L1 × 100%

[0098] In the formula, L1 is the total elongation; L2 is the remaining plastic elongation after unloading.

[0099] b. Repeated tensile fatigue performance: According to GB / T 36978-2018 "Determination of tensile elastic recovery rate of textiles - repeated tensile method", the sample was subjected to 10 cycles of 5% constant elongation tensile test, and the change of elastic recovery rate with the number of cycles was investigated to evaluate the fatigue resistance of the fiber.

[0100] c. The fibers prepared in Examples 4-6 and Comparative Examples 5-8 were washed 20 times according to the 4N procedure and hung to dry in accordance with GB / T 8629-2017 "Home Washing and Drying Procedures for Textile Testing". The elasticity retention rate was tested again. The test results are shown in Table 2.

[0101] Table 2: Statistical Table of Elastic Resilience Rate Test Data for Examples 4-6 and Comparative Examples 5-8

[0102]

[0103] As shown in Table 2, the experimental data show that the single elastic recovery rate, multiple elastic recovery rate, and elasticity retention rate after washing of Examples 4-6 are all above 90%, which is significantly higher than the relevant data of Comparative Examples 5-8, demonstrating good elastic recovery rate.

[0104] The foregoing has provided a detailed description of one embodiment of the present invention, but this description is merely a preferred embodiment and should not be construed as limiting the scope of the invention. All equivalent variations and modifications made within the scope of the claims of this invention should still fall within the patent coverage of this invention.

Claims

1. A process for the production of cool high stretch fibers, characterized by, The method comprises the following steps: cooling polyester POY filaments are subjected to elasticization process to obtain cooling high-elasticity fibers; the cooling polyester POY filaments are prepared by melt spinning of cooling master batches and polyester chips; the cooling master batches are prepared by melt blending of a modifier, an antioxidant and polyester chips; the preparation method of the modifier comprises the following steps: S1: yttrium nitrate, zirconium nitrate, erbium nitrate and deionized water are added into a reaction kettle A for dispersion, urea is added to adjust the pH to 3-6, the temperature is controlled at 120-150 DEG C, and the reaction is kept for 6-12 hours, then centrifugation, washing, drying, sintering and grinding are performed to obtain nanoparticles; S2: epoxy-modified hexagonal boron nitride powder, N,N-dimethylformamide and the nanoparticles are added into a reaction kettle B for dispersion, the temperature is controlled at 25-35 DEG C, and the reaction is kept for 8-12 hours, then centrifugation, washing and drying are performed to obtain core-shell particles; S3: in a nitrogen atmosphere, the core-shell particles, N,N-dimethylformamide, 4-carboxy-benzenesulfonyl azide and triphenylphosphine are added into a reaction kettle C, the temperature is controlled at 100-110 DEG C, the reaction is kept under stirring for 12-24 hours, then centrifugation, washing, drying and grinding are performed to obtain the modifier; The preparation method of the epoxy-modified hexagonal boron nitride powder comprises the following steps: h-BN powder, concentrated ammonia and isopropyl alcohol are added into a reaction bottle, the temperature is controlled at 0-5 DEG C, and the reaction is kept under stirring for 6-9 hours, then centrifugation is performed, the supernatant is taken and the pH of the supernatant is adjusted to 4-5, (3-glycidyloxypropyl) trimethoxysilane is added, the temperature is controlled at 50-60 DEG C, and the reaction is kept under stirring for 12-24 hours, then suction filtration, washing and drying are performed to obtain the epoxy-modified hexagonal boron nitride powder.

2. The process for preparing a cool high stretch fiber according to claim 1, characterized in that, The specific content of the elasticization process comprises the following steps: A1: the cooling polyester POY filaments are drawn into a pre-network nozzle for pre-networking treatment; A2: the filaments after the pre-networking treatment are drawn through a guide, a first roller, a first heat box for plasticization and heating, and stretching deformation; A3: the filaments after the stretching deformation are drawn into a false twister for false twisting; A4: the filaments after the false twisting are drawn into a main network nozzle for network processing; A5: the filaments after the network processing are drawn into a second heat box for heat setting; A6: the filaments after the heat setting are drawn through a third roller for drafting, an oiling roller for oiling, and finally a winding roller for winding to obtain the cooling high-elasticity fibers.

3. The process for preparing a cool high stretch fiber according to claim 2, characterized in that, The processing pressure of the pre-network nozzle is 0.04-0.05 MPa, the processing pressure of the main network nozzle is 0.12-0.16 MPa, the deformation temperature of the first heat box is 195-200 DEG C, the setting temperature of the second heat box is 85-95 DEG C, the D / Y ratio of the false twister is 1.65-1.85, the speed of the second roller is 700-800 m / min, the stretching multiple is 1.7-1.75, the setting overfeed rate is 4.9-5.4, and the winding overfeed rate is 4.1-4.

3.

4. The process for preparing a cool high stretch fiber according to claim 1, characterized in that, The mass ratio of the cool feeling master batch to polyester chip in the cool feeling polyester POY filament is 1-10:100; the master batch contains the following raw materials in percentage by weight: 0.5-10% modifier, 0.1-1% antioxidant, and the rest is polyester chip, and the sum of the percentages is 100%; the antioxidant is one or more of hindered phenolic antioxidant, triazole antioxidant, phosphite antioxidant, and sulfur ester antioxidant mixed in any ratio.

5. The method of claim 1, wherein the cool feeling high-elasticity fiber is prepared by the following steps: S1. mixing yttrium nitrate, zirconium nitrate, erbium nitrate, and deionized water in a ratio of 23.5-24 g: 10 g: 0.45-0.8 g: 500-1000 mL; S2. mixing the epoxy-modified hexagonal boron nitride powder, N,N-dimethylformamide, and nanoparticles in a ratio of 10-20 g: 200-400 mL: 10 g; S3. mixing the core-shell particles, N,N-dimethylformamide, 4-carboxy-benzenesulfonyl azide, and triphenylphosphine in a ratio of 10 g: 200-400 mL: 10-15 g: 0.1-1 g; and S4. mixing the mixture obtained in step S3 with the polyester chip in a ratio of 1-10:

100.

10. The method of any one of claims 1-7, wherein the cool feeling high-elasticity fiber is prepared by the following steps: S1. mixing yttrium nitrate, zirconium nitrate, erbium nitrate, and deionized water in a ratio of 23.5-24 g: 10 g: 0.45-0.8 g: 500-1000 mL; S2. mixing the epoxy-modified hexagonal boron nitride powder, N,N-dimethylformamide, and nanoparticles in a ratio of 10-20 g: 200-400 mL: 10 g; S3. mixing the core-shell particles, N,N-dimethylformamide, 4-carboxy-benzenesulfonyl azide, and triphenylphosphine in a ratio of 10 g: 200-400 mL: 10-15 g: 0.1-1 g; and S4. mixing the mixture obtained in step S3 with the polyester chip in a ratio of 1-10:

100.

6. The process for preparing a cool high stretch fiber according to claim 1, wherein 9. The cool feeling high-elasticity fiber of claim 8, wherein the fiber is applied to a fabric.

7. The process for preparing cool high stretch fiber according to claim 1, wherein the polyurethane prepolymer is prepared by reacting a diisocyanate compound with a diol compound in the presence of a chain extender. ​ 8. A cool high stretch fiber, characterized by, ​ ​

Citation Information

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