Far-infrared temperature-rising cotton-like nylon fabric and preparation method thereof

By adding composite far-infrared polymer powder and caprolactam to form a polyamide composite with covalent bonds in the spinning process, the problem of deterioration of fiber mechanical properties in the spinning process is solved, and a far-infrared temperature-rising cotton-like nylon fabric with high-efficiency far-infrared function, excellent mechanical properties and moisture absorption and quick-drying properties is achieved.

CN120520006BActive Publication Date: 2025-09-19SUZHOU GONGYEYUAN DISTRICTHEXIANG TEXTILE CO LTD
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Patent Information

Application Number
CN202511013639.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-07-23
Publication Date
2025-09-19
Estimated Expiration
2045-07-23

AI Technical Summary

Technical Problem

The existing spinning method adds far-infrared additives during the polymerization and spinning processes, which leads to the deterioration of the mechanical properties of the fiber.

Method used

Composite far-infrared polymer powder and caprolactam are covalently bonded in a polyamide composite, and nylon yarn is produced by melt spinning. Fluff is formed on the yarn surface to increase the cotton-like feel. The Si-O-Zr/Fe hybrid network and porous shell structure are used to enhance the infrared radiation efficiency and the moisture absorption and quick-drying properties of the fiber.

Benefits of technology

The fiber's far-infrared function and water-resistant performance are improved, the mechanical properties and moisture absorption and quick-drying properties are enhanced, and the velvety feel and warmth retention effect of the fabric are increased.

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Abstract

The present invention discloses a far-infrared temperature-rising cotton-like nylon fabric and a preparation method thereof, and relates to the field of functional fiber technology. The method comprises the following steps: spinning nylon yarn as at least one of the warp and weft yarns to produce a far-infrared temperature-rising cotton-like nylon fabric; the nylon yarn is produced by melt-spinning a polyamide composite; and the polyamide composite is obtained by connecting a composite far-infrared polymer powder to a polyamide molecular chain via a molecular chain bond. The composite far-infrared polymer powder prepared in this application is a core-shell particle with a porous structure on the surface. It is added to the polymerization process of caprolactam to connect it to the polyamide molecular chain via a molecular chain, effectively improving the functional water-resistant performance of the fabric. Moreover, the far-infrared polymer powder is compounded in the polyamide fiber to give the material an excellent far-infrared temperature-rising effect, so that the prepared fabric has the characteristics of good skin-friendly effect.
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Description

Technical Field

[0001] The invention relates to the technical field of functional fibers, in particular to a far-infrared temperature-rising cotton-like nylon fabric and a preparation method thereof. Background Art

[0002] As living standards improve, consumers' demands for clothing are shifting towards fashion and comfort. Cotton fabrics are widely used in clothing for their excellent moisture absorption, softness, and warmth. However, cotton, a key raw material in the textile industry, has seen its price rise. Due to its shortcomings in moisture conduction, stain and mildew resistance, low strength, and poor abrasion resistance, cotton fabrics are gradually being replaced in many applications by more cost-effective cotton-like synthetic fibers. At the same time, with the rapid development of new textile products and the chemical fiber industry, synthetic fibers are shifting towards natural, simulated, and functional fibers. Nylon, also known as polyamide fiber, is a major type of synthetic fiber. Due to the regular arrangement of nylon's molecular structure, numerous hydrogen bonds can form between macromolecules, resulting in high crystallinity and outstanding mechanical, chemical, and thermal properties. Nylon fabrics are the preferred material for some fabrics worn next to the skin. However, nylon's high moisture regain and rapid thermal conductivity can cause a cooling sensation on contact with the skin. These drawbacks are particularly pronounced in winter, limiting its use in winter.

[0003] Far-infrared fiber materials are used in clothing fabrics. The far-infrared ceramic particles contained in these materials convert radiation energy with wavelengths below 2μm into absorbed heat, which is then radiated toward the human body. However, they are reflective of radiation energy with wavelengths above 2μm. Leveraging this property, far-infrared fiber materials can repurpose much of the heat dissipated by the human body in the form of far-infrared radiation by absorbing, re-radiating, and reflecting it. The human body selectively absorbs far-infrared radiation, which, through molecular resonance, is transmitted to the subcutaneous layer, generating a warming effect. Far-infrared fibers are ideal materials for autumn and winter thermal insulation. The preparation of far-infrared fibers can be categorized into two main methods: coating and blend spinning. While the coating method is simple to operate, the resulting fibers exhibit poor hand feel and washability. The spinning method allows the addition of far-infrared additives during the polymerization and spinning processes to produce fibers with far-infrared temperature-raising properties. However, the incorporation of far-infrared additives deteriorates the mechanical properties of the fibers. Summary of the Invention

[0004] The purpose of the present invention is to provide a far-infrared temperature-rising cotton-like nylon fabric and a preparation method thereof, and to solve the following technical problems:

[0005] The existing spinning method adds far-infrared additives during the polymerization and spinning process, and obtains fibers with far-infrared temperature rise function through spinning. However, with the addition of far-infrared additives, the mechanical properties of the fibers deteriorate.

[0006] The purpose of the present invention can be achieved through the following technical solutions:

[0007] A method for preparing a far-infrared temperature-rising cotton-like nylon fabric comprises the following steps: spinning nylon yarn as at least one of warp yarn and weft yarn to prepare the far-infrared temperature-rising cotton-like nylon fabric;

[0008] Nylon yarn is produced by melt spinning of polyamide composites;

[0009] The specific preparation method of the polyamide composite comprises the following steps:

[0010] In a nitrogen atmosphere, the composite far-infrared polymer powder and molten caprolactam are added to a reaction bottle, the temperature is controlled at 110-120°C, the reaction is carried out for 1-2 hours, 6-aminocaproic acid is added, the temperature is controlled at 170-180°C, and the reaction is kept warm for 2-4 hours, the temperature is controlled at 260-270°C and the pressure is 0.3-0.5 MPa, and the reaction is kept warm for 3-6 hours, vacuum degassing, discharging, pelletizing, boiling, and vacuum drying are obtained to obtain a polyamide composite.

[0011] As a further solution of the present invention: the addition ratio of the composite far-infrared polymer powder, caprolactam, and 6-aminocaproic acid is 1-2g:100g:5-10g.

[0012] As a further solution of the present invention: the preparation method of the composite far-infrared polymer powder comprises the following steps:

[0013] A1: Add the template and ethanol solution to a reaction flask, control the temperature at 40-50°C, keep stirring for 0.5-1 hour, add tetraethyl orthosilicate, Zr(NO3)4·5H2O, and Fe(NO3)3·9H2O, adjust the pH to 3-4, keep hydrolyzing for 3-6 hours, add activated silicon carbide particles and disperse them evenly, control the temperature at 90-100°C, keep reacting for 24-36 hours, evaporate the solvent, and sinter at low temperature under a reducing atmosphere to obtain composite silicon carbide nanoparticles;

[0014] A2: Add composite silicon carbide nanoparticles, ethanol, and water into a reactor and disperse them evenly. Add γ-aminopropyltriethoxysilane, adjust the pH to 4-5, control the temperature at 60-70°C, react for 6-8 hours, vacuum dry, and heat treat to obtain composite far-infrared polymer powder.

[0015] As a further embodiment of the present invention, the particle size of the composite silicon carbide nanoparticles is 50-200 nm.

[0016] As a further embodiment of the present invention: the template in A1 is hexadecyltrimethylammonium bromide; the ethanol solution is 80vt% ethanol aqueous solution;

[0017] The addition ratio of the template, ethanol solution, tetraethyl orthosilicate, Zr(NO3)4·5H2O, Fe(NO3)3·9H2O, and activated silicon carbide particles is 2.4-3.6 g: 200-400 mL: 22.5-25 g: 4.8-7.2 g: 3.6-6 g: 100 g.

[0018] As a further solution of the present invention: the specific steps of low-temperature sintering under reducing atmosphere are: in 5% H2 / Ar premixed gas, heating rate 3-5°C / min, heating to 350-400°C, and calcining for 3-5h.

[0019] As a further solution of the present invention: the composite silicon carbide nanoparticles, ethanol and water in A2 are added to a reactor and dispersed evenly, and γ-aminopropyltriethoxysilane is added in a ratio of 10 g: 80-160 mL: 20-40 mL: 0.3-0.5 g.

[0020] As a further solution of the present invention: the specific steps of melt spinning are: melt spinning the polyamide compound through a twin-screw extruder; the processing temperature of the twin-screw extruder is 250-280°C.

[0021] As a further solution of the present invention: in the twin-screw extruder, the temperature in zone 1 is 255°C, zone 2 is 280°C, zone 3 is 275°C, zone 4 is 275°C, zone 5 is 275°C, zone 6 is 275°C, and zone 7 is 280°C.

[0022] As a further solution of the present invention, the nylon yarn is further subjected to air deformation before being woven into the fabric to achieve a cotton-like feel, so that fuzz is formed on the surface of the yarn to increase the velvety feel of the fabric.

[0023] As a further solution of the present invention, the far-infrared temperature-rising cotton-like nylon fabric is also blended with spandex yarn; the weight of the nylon yarn in the fabric accounts for 25-100% of the total weight of the fabric.

[0024] A far-infrared temperature-rising cotton-like nylon fabric is made by any of the above-mentioned preparation methods.

[0025] Beneficial effects of the present invention:

[0026] (1) This application first uses silicon carbide particles with high thermal conductivity and a far-infrared band (5-20μm) emissivity greater than 90% as cores, and uses tetraethyl orthosilicate, Zr(NO3)4·5H2O, and Fe(NO3)3·9H2O as raw materials to form a composite precursor with a Si-O-Zr / Fe hybrid network through a sol-gel method; the composite precursor is used to form a porous shell layer on the surface of the silicon carbide particles to obtain composite silicon carbide nanoparticles; and then it is subjected to amino treatment using γ-aminopropyltriethoxysilane to obtain a composite far-infrared polymer powder. This application adds the composite far-infrared polymer powder to the ring-opening polymerization process of caprolactam, and uses the amino groups on the surface of the composite far-infrared polymer powder to undergo amidation reaction with the carboxyl groups of the nylon prepolymer to form a covalent bond connection, thereby obtaining polyamide composite pellets. The pellets are melt-spun to obtain nylon yarn.

[0027] The present application adds tetraethyl orthosilicate to the composite precursor to enhance the hydrolysis resistance of the composite far-infrared polymer powder. The present application adds Zr(NO3)4·5H2O to the composite precursor to make the shell have the characteristics of high refractive index and enhanced infrared reflection. The present application adds Fe(NO3)3·9H2O to the composite precursor to enhance the hydrolysis resistance of the composite far-infrared polymer powder. 3+ The dd transition enhances visible light absorption, producing a synergistic temperature rise with far-infrared radiation. Furthermore, the addition of the transition metal Fe achieves lattice doping, effectively broadening the far-infrared radiation band. This application also incorporates a template agent into the composite precursor to impart a porous shell structure. The metal doping (Zr / Fe) and the porous shell structure synergistically enhance infrared radiation efficiency. The porous shell structure also improves the fiber's moisture absorption and quick-drying properties.

[0028] (2) The present application adds composite far-infrared polymer powder during the polymerization of caprolactam, which not only makes the resulting nylon yarn have far-infrared function, but also bonds the composite far-infrared polymer powder to the polyamide molecular chain, effectively improving the washability of the far-infrared function. The present application also uses air deformation to treat the melt-spun nylon yarn to imitate the cotton feel, forming fuzz on the yarn surface to increase the velvety feel of the fabric, effectively increase the fluffiness of the fabric itself, increase the thickness of the air layer, reduce the direct conduction of human body heat to the outside, and achieve the purpose of heat retention.

[0029] (3) The present application also sintered the silicon carbide attached with composite metal oxides at low temperature in a reducing atmosphere to obtain composite silicon carbide nanoparticles; the reducing atmosphere can effectively reduce the iron oxide in the shell to ferroferric oxide, thereby enhancing the magnetic properties and improving the thermal conductivity, and also improving the integrity of the shell pores; the reducing atmosphere can also prevent the silicon carbide particles from being oxidized during the calcination process.

[0030] (4) The present application deposits a shell layer with a mesoporous structure on the surface of silicon carbide particles, which effectively increases the specific surface area and enhances the reaction activity of subsequent organic modification. The porous shell structure of the particles can also allow the polyamide molecular chains to intersperse and grow, thereby improving the peeling strength between the particles and the molecular chains.

[0031] (5) The present invention performs activation treatment on the silicon carbide particles before the shell layer deposition, which effectively increases the hydroxyl content on the particle surface, facilitates the grafting of tetraethyl orthosilicate onto the silicon carbide surface, and facilitates the subsequent deposition of the composite precursor. DETAILED DESCRIPTION

[0032] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0033] Example 1: The preparation method of composite far-infrared polymer powder comprises the following steps:

[0034] A1: Immerse silicon carbide particles in 3 mol / L nitric acid solution, stir magnetically at 80°C for 2 h, wash with water until neutral, and vacuum dry at 120°C for 6 h to obtain activated silicon carbide particles;

[0035] A2: 2.4 g of hexadecyltrimethylammonium bromide and 200 mL of 80% ethanol aqueous solution were added to a reaction flask, the temperature was controlled at 40°C, and the mixture was stirred for 0.5 h. 22.5 g of tetraethyl orthosilicate, 4.8 g of Zr(NO3)4·5H2O, and 3.6 g of Fe(NO3)3·9H2O were added, the pH was adjusted to 3.5, and the mixture was hydrolyzed for 3 h. 100 g of activated silicon carbide particles were added and dispersed evenly. The temperature was controlled at 90°C and the reaction was kept warm for 24 h. The solvent was evaporated, and the mixture was heated to 350°C under 5% H2 / Ar premix at a heating rate of 3°C / min and calcined for 3 h to obtain composite silicon carbide nanoparticles.

[0036] A3: Add 10 g of composite silicon carbide nanoparticles, 80 mL of ethanol, and 20 mL of water into a reactor and disperse them evenly. Add 0.3 g of γ-aminopropyltriethoxysilane, adjust the pH to 4, control the temperature at 60°C, react for 6 h, vacuum dry (control the temperature at 80°C for 12 h), and heat treat (control the temperature at 120°C for 30 min) to obtain a composite far-infrared polymer powder.

[0037] Example 2: The preparation method of composite far-infrared polymer powder comprises the following steps:

[0038] A1: Immerse silicon carbide particles in 3 mol / L nitric acid solution, stir magnetically at 80°C for 2 h, wash with water until neutral, and vacuum dry at 120°C for 6 h to obtain activated silicon carbide particles;

[0039] A2: 3 g of hexadecyltrimethylammonium bromide and 300 mL of 80% ethanol aqueous solution were added to a reaction flask, the temperature was controlled at 45°C, and the mixture was stirred for 0.5 h. 22.5 g of tetraethyl orthosilicate, 5 g of Zr(NO3)4·5H2O, and 4.5 g of Fe(NO3)3·9H2O were added, the pH was adjusted to 3.5, and the mixture was hydrolyzed for 4 h. 100 g of activated silicon carbide particles were added and dispersed evenly. The temperature was controlled at 95°C and the reaction was kept warm for 30 h. The solvent was evaporated, and the mixture was heated to 350°C under 5% H2 / Ar premix at a heating rate of 3°C / min and calcined for 4 h to obtain composite silicon carbide nanoparticles.

[0040] A3: Add 10 g of composite silicon carbide nanoparticles, 120 mL of ethanol, and 30 mL of water into a reactor and disperse them evenly. Add 0.4 g of γ-aminopropyltriethoxysilane, adjust the pH to 4, control the temperature at 70°C, react for 6 h, vacuum dry (control the temperature at 80°C for 12 h), and heat treat (control the temperature at 120°C for 30 min) to obtain a composite far-infrared polymer powder.

[0041] Example 3: The preparation method of composite far-infrared polymer powder comprises the following steps:

[0042] A1: Immerse silicon carbide particles in 3 mol / L nitric acid solution, stir magnetically at 80°C for 2 h, wash with water until neutral, and vacuum dry at 120°C for 6 h to obtain activated silicon carbide particles;

[0043] A2: 3.6 g of hexadecyltrimethylammonium bromide and 400 mL of 80% ethanol aqueous solution were added to a reaction flask, the temperature was controlled at 50°C, and the mixture was stirred for 1 h. 25 g of tetraethyl orthosilicate, 7.2 g of Zr(NO3)4·5H2O, and 6 g of Fe(NO3)3·9H2O were added, the pH was adjusted to 4, and the mixture was hydrolyzed for 6 h. 100 g of activated silicon carbide particles were added and dispersed evenly. The temperature was controlled at 100°C and the reaction was kept at this temperature for 24 h. The solvent was evaporated, and the mixture was heated to 400°C under 5% H2 / Ar premix at a heating rate of 5°C / min and calcined for 4 h to obtain composite silicon carbide nanoparticles.

[0044] A3: Add 10 g of composite silicon carbide nanoparticles, 160 mL of ethanol, and 40 mL of water into a reactor and disperse them evenly. Add 0.5 g of γ-aminopropyltriethoxysilane, adjust the pH to 5, control the temperature at 70°C, react for 8 h, vacuum dry (control the temperature at 80°C for 12 h), and heat treat (control the temperature at 120°C for 30 min) to obtain a composite far-infrared polymer powder.

[0045] Example 4: A method for preparing a far-infrared temperature-rising cotton-like nylon fabric, comprising the following steps:

[0046] S1: In a nitrogen atmosphere, 2 g of the composite far-infrared polymer powder prepared in Example 1 and 100 g of molten caprolactam (100 ° C) were added to a reaction flask, the temperature was controlled at 110 ° C, the reaction was continued for 1 h, 5 g of 6-aminocaproic acid was added, the temperature was controlled at 170 ° C, the reaction was kept warm for 2 h, the temperature was controlled at 260 ° C, the pressure was 0.3 MPa, the reaction was kept warm for 3 h, vacuum degassing (-0.095 MPa, 30 min) was performed, pelletized, boiled, and vacuum dried to obtain a polyamide composite;

[0047] S2: melt-spinning the polyamide composite through a twin-screw extruder at 255° C. in zone 1, 280° C. in zone 2, 275° C. in zone 3, 275° C. in zone 4, 275° C. in zone 5, 275° C. in zone 6, and 280° C., and drawing and heat-setting the composite on a four-roller drawing machine at a temperature of 100° C. to obtain nylon filaments;

[0048] S3: The nylon filaments are subjected to air deformation to achieve a cotton-like feel, thereby obtaining nylon yarn;

[0049] S4: Nylon / spandex weft-knitted double-sided fabric with a blending ratio of 75 / 25, made into 230g / m 2 Far infrared temperature rising cotton-like nylon fabric.

[0050] Example 5: A method for preparing a far-infrared temperature-rising cotton-like nylon fabric, comprising the following steps:

[0051] S1: In a nitrogen atmosphere, 2g of the composite far-infrared polymer powder prepared in Example 2 and 100g of molten caprolactam (100°C) were added to a reaction flask, the temperature was controlled at 120°C, the reaction was carried out for 1.5h, 5g of 6-aminocaproic acid was added, the temperature was controlled at 180°C, the reaction was kept warm for 2h, the temperature was controlled at 270°C and the pressure was 0.4MPa, the reaction was kept warm for 4.5h, vacuum degassing (-0.095MPa, 30min) was performed, the material was pelletized, boiled in water, and vacuum dried to obtain a polyamide composite;

[0052] S2: melt-spinning the polyamide composite through a twin-screw extruder at 255° C. in zone 1, 280° C. in zone 2, 275° C. in zone 3, 275° C. in zone 4, 275° C. in zone 5, 275° C. in zone 6, and 280° C., and drawing and heat-setting the composite on a four-roller drawing machine at a temperature of 100° C. to obtain nylon filaments;

[0053] S3: The nylon filaments are subjected to air deformation to achieve a cotton-like feel, thereby obtaining nylon yarn;

[0054] S4: Nylon / spandex weft-knitted double-sided fabric with a blending ratio of 75 / 25, made into 230g / m 2 Far infrared temperature rising cotton-like nylon fabric.

[0055] Example 6: A method for preparing a far-infrared temperature-rising cotton-like nylon fabric, comprising the following steps:

[0056] S1: In a nitrogen atmosphere, 2g of the composite far-infrared polymer powder prepared in Example 3 and 100g of molten caprolactam (100°C) were added to a reaction flask, the temperature was controlled at 110°C, the reaction was continued for 2h, 5g of 6-aminocaproic acid was added, the temperature was controlled at 180°C, the reaction was kept warm for 4h, the temperature was controlled at 270°C and the pressure was 0.3MPa, the reaction was kept warm for 3h, vacuum degassing (-0.095MPa, 30min) was performed, the material was pelletized, boiled in water, and vacuum dried to obtain a polyamide composite;

[0057] S2: The polyamide composite is melt-spun through a twin-screw extruder, with the temperatures of zone 1 at 255°C, zone 2 at 280°C, zone 3 at 275°C, zone 4 at 275°C, zone 5 at 275°C, zone 6 at 275°C, and zone 7 at 280°C, and is drawn and heat-set on a four-roller draw-off machine with a hot roller set at 100°C, with an apparent stretching ratio of 4 to obtain nylon filaments;

[0058] S3: The nylon filaments are subjected to air deformation to achieve a cotton-like feel, thereby obtaining nylon yarn;

[0059] S4: Nylon / spandex weft-knitted double-sided fabric with a blending ratio of 75 / 25, made into 230g / m 2 Far infrared temperature rising cotton-like nylon fabric.

[0060] Comparative Example 1: The preparation method of composite far-infrared polymer powder comprises the following steps:

[0061] A1: Immerse silicon carbide particles in 3 mol / L nitric acid solution, stir magnetically at 80°C for 2 h, wash with water until neutral, and vacuum dry at 120°C for 6 h to obtain activated silicon carbide particles;

[0062] A2: Add 3 g of hexadecyltrimethylammonium bromide and 300 mL of 80% ethanol aqueous solution to a reaction flask, control the temperature at 45°C, and stir for 0.5 h. Then add 22.5 g of tetraethyl orthosilicate, 5 g of Zr(NO3)4·5H2O, and 4.5 g of Fe(NO3)3·9H2O, adjust the pH to 3.5, and hydrolyze for 4 h. Then add 100 g of activated silicon carbide particles and disperse them evenly. Control the temperature at 95°C and react for 30 h. Evaporate the solvent, and heat the mixture to 350°C under 5% H2 / Ar premix at a heating rate of 3°C / min. Then calcine for 4 h to obtain a composite far-infrared polymer powder.

[0063] Comparative Example 2: The preparation method of composite far-infrared polymer powder comprises the following steps:

[0064] A1: Immerse silicon carbide particles in 3 mol / L nitric acid solution, stir magnetically at 80°C for 2 h, wash with water until neutral, and vacuum dry at 120°C for 6 h to obtain activated silicon carbide particles;

[0065] A2: Add 22.5 g of tetraethyl orthosilicate, 5 g of Zr(NO3)4·5H2O, 4.5 g of Fe(NO3)3·9H2O, and 300 mL of 80% ethanol aqueous solution, control the temperature to 45°C, keep stirring for 0.5 h, adjust the pH to 3.5, keep hydrolyzing for 4 h, add 100 g of activated silicon carbide particles and disperse them evenly, control the temperature to 95°C, keep the reaction for 30 h, evaporate the solvent, and heat the mixture to 350°C under 5% H2 / Ar premix at a heating rate of 3°C / min and calcine for 4 h to obtain composite silicon carbide nanoparticles;

[0066] A3: Add 10 g of composite silicon carbide nanoparticles, 120 mL of ethanol, and 30 mL of water into a reactor and disperse them evenly. Add 0.4 g of γ-aminopropyltriethoxysilane, adjust the pH to 4, control the temperature at 70°C, react for 6 h, vacuum dry (control the temperature at 80°C for 12 h), and heat treat (control the temperature at 120°C for 30 min) to obtain a composite far-infrared polymer powder.

[0067] Comparative Example 3: The preparation method of composite far-infrared polymer powder comprises the following steps:

[0068] A1: Immerse silicon carbide particles in 3 mol / L nitric acid solution, stir magnetically at 80°C for 2 h, wash with water until neutral, and vacuum dry at 120°C for 6 h to obtain activated silicon carbide particles;

[0069] A2: Add 3 g of hexadecyltrimethylammonium bromide and 300 mL of 80% ethanol aqueous solution to a reaction flask, control the temperature at 45°C, keep stirring for 0.5 h, add 22.5 g of tetraethyl orthosilicate, 5 g of Zr(NO3)4·5H2O, and 4.5 g of Fe(NO3)3·9H2O, adjust the pH to 3.5, keep hydrolyzing for 4 h, add 100 g of activated silicon carbide particles and disperse them evenly, control the temperature at 95°C, keep reacting for 30 h, evaporate the solvent, increase the temperature to 500°C at a rate of 3°C / min, and calcine for 4 h to obtain composite silicon carbide nanoparticles;

[0070] A3: Add 10 g of composite silicon carbide nanoparticles, 120 mL of ethanol, and 30 mL of water into a reactor and disperse them evenly. Add 0.4 g of γ-aminopropyltriethoxysilane, adjust the pH to 4, control the temperature at 70°C, react for 6 h, vacuum dry (control the temperature at 80°C for 12 h), and heat treat (control the temperature at 120°C for 30 min) to obtain a composite far-infrared polymer powder.

[0071] Comparative Example 4: The preparation method of composite far-infrared polymer powder comprises the following steps:

[0072] A1: Immerse silicon carbide particles in 3 mol / L nitric acid solution, stir magnetically at 80°C for 2 h, wash with water until neutral, and vacuum dry at 120°C for 6 h to obtain activated silicon carbide particles;

[0073] A2: 22.5 g of tetraethyl orthosilicate, 5 g of Zr(NO3)4·5H2O, 4.5 g of Fe(NO3)3·9H2O, and 300 mL of 80% ethanol aqueous solution were added to a reaction flask. The temperature was controlled at 45°C and the mixture was stirred for 0.5 h. The pH was adjusted to 3.5 and the mixture was hydrolyzed for 4 h. The solvent was evaporated and the mixture was heated to 350°C at a rate of 3°C / min under 5% H2 / Ar premixed gas and calcined for 4 h to obtain composite particles.

[0074] A3: The composite particles prepared in step A2 were mixed with 100 g of activated silicon carbide particles and anhydrous ethanol to prepare a slurry with a solid content of 15 wt%. The slurry was ball-milled, aged for 12 h, and dried to obtain composite silicon carbide nanoparticles.

[0075] A4: Add 10 g of composite silicon carbide nanoparticles, 120 mL of ethanol, and 30 mL of water into a reactor and disperse them evenly. Add 0.4 g of γ-aminopropyltriethoxysilane, adjust the pH to 4, control the temperature to 70°C, react for 6 h, vacuum dry (control the temperature at 80°C for 12 h), and heat treat (control the temperature at 120°C for 30 min) to obtain a composite far-infrared polymer powder.

[0076] Comparative Example 5: Compared with Example 5, Comparative Example 5 only replaces the composite far-infrared polymer powder prepared in Example 2 added in Example 5 with the composite far-infrared polymer powder prepared in Comparative Example 1 in equal amount, and the remaining components and preparation method are exactly the same as those in Example 5.

[0077] Comparative Example 6: Compared with Example 5, Comparative Example 6 only replaces the composite far-infrared polymer powder prepared in Example 2 added in Example 5 with the composite far-infrared polymer powder prepared in Comparative Example 2. The remaining components and preparation methods are exactly the same as those in Example 5.

[0078] Comparative Example 7: Compared with Example 5, Comparative Example 7 only replaces the composite far-infrared polymer powder prepared in Example 2 added in Example 5 with the composite far-infrared polymer powder prepared in Comparative Example 3. The remaining components and preparation methods are exactly the same as those in Example 5.

[0079] Comparative Example 8: Compared with Example 5, Comparative Example 8 only replaces the composite far-infrared polymer powder prepared in Example 2 added in Example 5 with the composite far-infrared polymer powder prepared in Comparative Example 4. The remaining components and preparation methods are exactly the same as those in Example 5.

[0080] Performance testing

[0081] (1) Far infrared performance: According to GB / T 30127-2013 “Testing and evaluation of far infrared performance of textiles”, the far infrared performance of the fabric was measured using a far infrared radiation temperature rise tester. The test results are shown in Table 1. According to the 5A procedure of GB / T 8629-2001 “Household washing and drying procedures for textile testing”, the fabric was washed 50 times and dried in an oven, and then tested again. The test results are shown in Table 1.

[0082] Table 1: Far infrared performance test data statistics

[0083]

[0084] As can be seen from Table 1, the fabric woven from the fibers prepared in the present application has a far-infrared emissivity of not less than 0.88 and a far-infrared radiation temperature rise of not less than 1.4°C, and has far-infrared properties.

[0085] (2) Mechanical properties: The mechanical properties of the nylon yarns prepared in Examples 4-6 and Comparative Examples 5-8 were tested using a multifilament strength tester with a gauge length of 250 mm to test the breaking strength and elongation of the materials. The test results are shown in Table 2.

[0086] (3) Moisture absorption and quick-drying performance: The fabrics prepared in Examples 4-6 and Comparative Examples 5-8 were used as samples. The evaporation rate of the fabric samples was measured according to GB / T21655.1-2008 "Evaluation of Moisture Absorption and Quick-drying Properties Part 1: Single Item Combination Test Method". The test results are shown in Table 2.

[0087] Table 2: Mechanical properties test data statistics

[0088]

[0089] As can be seen from Table 2, the composite far-infrared polymer powder prepared in the present application is added to polyamide, and the hydrophilic groups and porous structure on the surface of the composite far-infrared polymer powder effectively improve the moisture absorption and quick-drying properties of the polyamide; and the composite far-infrared polymer powder is chemically bonded to the polyamide molecular chain, which effectively avoids the direct addition of the composite far-infrared polymer powder resulting in a decrease in the mechanical properties of the material, thereby giving the material excellent mechanical properties.

[0090] The above is a detailed description of an embodiment of the present invention. However, the content described is only a preferred embodiment of the present invention and should not be considered to limit the scope of the present invention. All equivalent changes and improvements made within the scope of the present invention should still fall within the scope of the patent coverage of the present invention.

Claims

1. A method for preparing far-infrared temperature-rising cotton-like nylon fabric, characterized in that: The method comprises the following steps: spinning nylon yarn as at least one of warp yarn and weft yarn to prepare far-infrared temperature-rising cotton-like nylon fabric; The nylon yarn is produced by melt spinning of a polyamide composite; The specific preparation method of the polyamide composite comprises the following steps: In a nitrogen atmosphere, the composite far-infrared polymer powder and molten caprolactam are added to a reaction bottle, the temperature is controlled at 110-120°C, the reaction is carried out for 1-2 hours, 6-aminocaproic acid is added, the temperature is controlled at 170-180°C, and the reaction is kept warm for 2-4 hours, the temperature is controlled at 260-270°C and the pressure is 0.3-0.5 MPa, the reaction is kept warm for 3-6 hours, vacuum degassing, discharging, pelletizing, boiling, and vacuum drying are obtained to obtain a polyamide composite; The preparation method of the composite far-infrared polymer powder comprises the following steps: A1: Add the template and ethanol solution to a reaction flask, control the temperature at 40-50°C, keep stirring for 0.5-1 hour, add tetraethyl orthosilicate, Zr(NO3)4·5H2O, and Fe(NO3)3·9H2O, adjust the pH to 3-4, keep hydrolyzing for 3-6 hours, add activated silicon carbide particles and disperse them evenly, control the temperature at 90-100°C, keep reacting for 24-36 hours, evaporate the solvent, and sinter at low temperature under a reducing atmosphere to obtain composite silicon carbide nanoparticles; A2: Add composite silicon carbide nanoparticles, ethanol, and water into a reactor and disperse them evenly. Add γ-aminopropyltriethoxysilane, adjust the pH to 4-5, control the temperature at 60-70°C, react for 6-8 hours, vacuum dry, and heat treat to obtain composite far-infrared polymer powder.

2. The method for preparing a far-infrared temperature-rising cotton-like nylon fabric according to claim 1, characterized in that: The addition ratio of the composite far-infrared polymer powder, caprolactam and 6-aminocaproic acid is 1-2g:100g:5-10g.

3. The method for preparing a far-infrared temperature-rising cotton-like nylon fabric according to claim 2, characterized in that: The template agent in A1 is hexadecyltrimethylammonium bromide; the ethanol solution is 80vt% ethanol aqueous solution; The addition ratio of the template, ethanol solution, tetraethyl orthosilicate, Zr(NO3)4·5H2O, Fe(NO3)3·9H2O, and activated silicon carbide particles is 2.4-3.6 g: 200-400 mL: 22.5-25 g: 4.8-7.2 g: 3.6-6 g: 100 g.

4. The method for preparing a far-infrared temperature-rising cotton-like nylon fabric according to claim 2, characterized in that: The composite silicon carbide nanoparticles, ethanol and water in A2 are added to a reactor and dispersed evenly, and γ-aminopropyltriethoxysilane is added in a ratio of 10 g: 80-160 mL: 20-40 mL: 0.3-0.5 g.

5. The method for preparing a far-infrared temperature-rising cotton-like nylon fabric according to claim 1, characterized in that: The specific steps of melt spinning are: melt spinning the polyamide compound through a twin-screw extruder; the processing temperature of the twin-screw extruder is 250-280°C.

6. The method for preparing a far-infrared temperature-rising cotton-like nylon fabric according to claim 1, characterized in that: The nylon yarn is further subjected to air deformation before being woven into the fabric to achieve a cotton-like feel.

7. The method for preparing a far-infrared temperature-rising cotton-like nylon fabric according to claim 1, characterized in that: The far-infrared temperature-rising cotton-like nylon fabric is also blended with spandex yarn; the weight of the nylon yarn in the fabric accounts for 75-100% of the total weight of the fabric.

8. A far-infrared temperature-rising cotton-like nylon fabric, characterized in that: Prepared by the preparation method according to any one of claims 1 to 7.

Citation Information

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