Soft skin-friendly fabric and preparation method thereof

The fabric combines modified polyester, silica microspheres, and hydrogen-containing silicone oil to address softness and skin-friendliness issues, achieving enhanced comfort, antibacterial, and flame-retardant properties through electrostatic spinning and polymerization processes.

CN119145080AInactive Publication Date: 2024-12-17NANTONG JIAYUSI TEXTILE GROUP
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Patent Information

Application Number
CN202411621893.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-14
Publication Date
2024-12-17
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

Existing fabrics fail to meet the requirements of high-end consumers for softness, skin-friendliness, and comfort, leading to friction, skin irritation, and moisture retention issues.

Method used

A soft and skin-friendly fabric is produced by electrostatically spinning a mixture of modified polyester, modified silicon dioxide microspheres, and hydrogen-containing silicone oil, utilizing silver-loaded porous silica microspheres, formaldehyde-modified bamboo cellulose, and 2,6-pyridinedimethylamine to enhance antibacterial and skin-friendly properties, and incorporating a triazine structure for flame retardancy.

Benefits of technology

The fabric exhibits improved softness, skin-friendliness, antibacterial properties, flame retardancy, and mechanical properties, with enhanced moisture retention and reduced friction, while maintaining comfort and durability.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a soft skin-friendly fabric and a preparation method thereof, and relates to the field of textile fabrics. When the soft skin-friendly fabric is prepared, silver ions are loaded on ethyl orthosilicate through a template method to obtain silver-loaded porous silicon dioxide microspheres; polymerizing and depositing the aldehyde bamboo cellulose, 2, 6-pyridine dimethylamine and 2-vinyl-4, 6-diamino-1, 3, 5-triazine on the surfaces of the silver-loaded porous silicon dioxide microspheres to obtain modified porous silicon dioxide microspheres; polymerizing terephthalic acid, vinyl terephthalic acid, ethylene glycol and N-methyldiethanolamine to obtain pre-modified polyester powder; the pre-modified polyester powder and 4-(bromomethyl)-2, 6-di-tert-butylphenol are subjected to a reaction, and modified polyester is obtained; the modified polyester, the modified silicon dioxide microspheres and hydrogen-containing silicone oil are mixed and subjected to electrostatic spinning, and then the soft and skin-friendly fabric is obtained through spinning. The prepared soft skin-friendly fabric has excellent soft skin-friendly, antibacterial, anti-aging, antistatic, flame-retardant and mechanical properties.
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Description

Technical Field

[0001] The invention relates to the field of textile fabrics, in particular to a soft, skin-friendly fabric and a preparation method thereof. Background Art

[0002] With the development of society and economy, people's living standards are constantly improving. High-end consumers have put forward a series of requirements for fabrics, such as softness, skin-friendly and comfortable. However, it is difficult to meet the above requirements of consumers by using chemical agents as modifiers to finish fabrics. Improving softness and skin-friendly properties not only makes the fabric more comfortable, but also reduces the friction on the surface of the fabric, avoids irritation to the skin during contact, better maintains the moisture of the skin, and reduces skin dryness and allergies. Therefore, the development of fabrics with good softness and skin-friendly properties has broad market prospects. Summary of the invention

[0003] The object of the present invention is to provide a soft, skin-friendly fabric and a preparation method thereof, so as to solve the problems existing in the prior art.

[0004] In order to solve the above technical problems, the present invention provides the following technical solutions: A soft and skin-friendly fabric is obtained by electrostatically spinning a mixture of modified polyester, modified silicon dioxide microspheres and hydrogen-containing silicone oil.

[0005] As an optimization, the hydrogen-containing silicone oil model is KF99, which comes from Shenzhen Jipeng Silicone Fluoride Materials Co., Ltd.

[0006] As an optimization, the modified polyester is obtained by polymerizing terephthalic acid, vinyl terephthalic acid, ethylene glycol and N-methyldiethanolamine and then reacting with 4-(bromomethyl)-2,6-di-tert-butylphenol.

[0007] As an optimization, the modified silica microspheres are obtained by loading silver ions onto tetraethyl orthosilicate and then polymerizing and depositing aldehyde-modified bamboo cellulose, 2,6-pyridinedimethylamine and 2-vinyl-4,6-diamino-1,3,5-triazine on the surface.

[0008] A method for preparing a soft, skin-friendly fabric comprises the following steps: (1) Mix 0.07~0.08 mol / L silver nitrate aqueous solution and template dispersion in a volume ratio of 1:(0.5~1.5), stir at 20~30℃ and 100~200 rpm for 55~65 min, add 0.3~0.5 times the volume of silver nitrate aqueous solution and 0.07~0.08 g / L polyvinyl pyrrolidone alcohol solution, continue stirring for 1~3 h, add 0.05~0.07 times the volume of silver nitrate aqueous solution and ammonia water. Stirring at 200-300 rpm for 55-65 min, adding 0.01-0.03 times the volume of the silver nitrate aqueous solution of tetraethyl orthosilicate at a uniform rate within 20-30 min, continuing stirring for 1-3 h and filtering, washing with deionized water 3-5 times, drying at 55-65° C. for 10-12 h, heating to 500-600° C. at a rate of 0.5-1.5° C. / min and keeping the temperature for 5-7 h, and naturally cooling to room temperature to obtain silver-loaded porous silica microspheres; (2) The formaldehyde-modified bamboo cellulose, silver-loaded porous silica microspheres and N,N-dimethylformamide were mixed in a mass ratio of 1:(2-3):(199-201), stirred at 20-30°C and 200-300 rpm for 20-30 min, 2,6-pyridinedimethylamine with a molar amount of 0.4-0.6 times the aldehyde group in the formaldehyde-modified bamboo cellulose and 2-vinyl-4,6-diamino-1,3,5-triazine with a molar amount of 0.4-0.6 times the aldehyde group in the formaldehyde-modified bamboo cellulose were added, the temperature was raised to 75-85°C and stirring was continued for 2-4 h, the mixture was naturally cooled to room temperature and filtered, washed with deionized water for 3-5 times, and dried at 65-75°C for 10-12 h to obtain modified porous silica microspheres; (3) Mix terephthalic acid, vinyl terephthalic acid, ethylene glycol, N-methyldiethanolamine and antimony acetate in a mass ratio of 1: (0.3~0.4): (1.3~1.4): (0.3~0.5): (0.01~0.02), stir for 3~5 hours in a nitrogen atmosphere at 210~220°C, 400~500rpm, and 0.02~0.04MPa, reduce the pressure to 50~100Pa and continue stirring for 10~20min, raise the temperature to 255~265°C and 45~55Pa and continue the reaction for 1~2 hours. h, pour into deionized water, cool and take out pellets, grind and sieve 80-100 mesh to obtain pre-modified polyester powder; mix the pre-modified polyester powder, 4-(bromomethyl)-2,6-di-tert-butylphenol and dichloromethane in a mass ratio of 1:(0.5-0.6):(19-21), stir at 75-85°C and 200-300rpm for 5-7h under nitrogen environment, cool naturally to room temperature and filter, wash with saturated salt water and deionized water for 3-5 times respectively, and dry at 55-65°C for 8-10h to obtain modified polyester; (4) The modified polyester, modified silica microspheres, hydrogenated silicone oil, trifluoroacetic acid and dichloromethane were mixed in a mass ratio of 1:(0.15-0.17):(1-2):(4.3-4.5):(0.9-1.3), stirred at 20-30°C and 200-300 rpm for 3-5 h, 0.01-0.02 times the mass of the modified polyester was added with chloroplatinic acid, and the stirring was continued for 10-20 min. The mixture was allowed to stand for 10-20 min, and electrospinning was performed under the conditions of a spinning voltage of 27-29 kV, a receiving distance of 14-16 cm, and a spinning solution push rate of 0.002-0.004 mm / s. After completion, the mixture was allowed to stand at 60-70°C for 6-8 h, washed with deionized water for 3-5 times, and dried at 55-65°C for 8-10 h to obtain spun fibers. The spun fibers were spun and woven by a textile machine to obtain soft and skin-friendly fabrics.

[0009] As an optimization, the template dispersion in step (1) is prepared by mixing polystyrene microsphere powder and 70-80% sulfuric acid solution in a mass ratio of 1:(33-34), ultrasonically dispersing at 35-45° C. for 40-50 min, naturally cooling to room temperature and then centrifuging, washing with anhydrous ethanol for 3-5 times, adding anhydrous ethanol in an amount of 95-105 times the mass of the polystyrene microsphere powder, and stirring at 20-30° C. and 200-300 rpm for 1-2 h.

[0010] As an optimization, the polystyrene microsphere powder comes from Dongguan Xiuzhisheng Plastic Co., Ltd.

[0011] As an optimization, the aldehyde-modified bamboo cellulose in step (2) is prepared by mixing bamboo fiber powder, sodium periodate and deionized water in a mass ratio of 1:(3-5):(3-5), adjusting the pH value to 3-5 with a hydrochloric acid solution having a mass fraction of 16-18%, stirring for 28-32 hours at 20-30° C. and 150-250 r / min under light-proof conditions, adding ethylene glycol in an amount of 1.4-1.6 times the mass of the bamboo fiber powder, continuing to stir for 1-2 hours, filtering, washing with deionized water for 3-5 times, and drying at 45-55° C. for 23-25 ​​hours.

[0012] As an optimization, the bamboo fiber powder comes from Shanggao County Polysilicon Mining Co., Ltd.

[0013] As an optimization, the reaction equation for the aldehyde-modified bamboo cellulose in step (2) is: .

[0014] As an optimization, the reaction equation for modifying the porous silica microspheres in step (2) is: .

[0015] As an optimization, the reaction equation of the pre-modified polyester in step (3) is: ; Where R1 is: or .

[0016] As an optimization, the reaction equation of the modified polyester in step (3) is: ; Where R1 is: or .

[0017] Compared with the prior art, the beneficial effects achieved by the present invention are: When preparing a soft and skin-friendly fabric, the present invention loads silver ions onto tetraethyl orthosilicate through a template method to obtain silver-loaded porous silica microspheres; then, formaldehyde-modified bamboo cellulose, 2,6-pyridinedimethylamine and 2-vinyl-4,6-diamino-1,3,5-triazine are polymerized and deposited on the surface of the silver-loaded porous silica microspheres to obtain modified porous silica microspheres; terephthalic acid, vinyl terephthalic acid, ethylene glycol and N-methyldiethanolamine are polymerized to obtain pre-modified polyester powder; then, the pre-modified polyester powder and 4-(bromomethyl)-2,6-di-tert-butylphenol are reacted to obtain modified polyester; and the modified polyester, modified silica microspheres and hydrogen-containing silicone oil are mixed and electrostatically spun and then woven to obtain the soft and skin-friendly fabric.

[0018] Firstly, silver ions are loaded onto tetraethyl orthosilicate by a template method to obtain silver-loaded porous silica microspheres; then, formaldehyde-modified bamboo cellulose, 2,6-pyridinedimethylamine and 2-vinyl-4,6-diamino-1,3,5-triazine are polymerized and deposited on the surface of the silver-loaded porous silica microspheres to obtain modified porous silica microspheres; porous silica microspheres loaded with silver ions are prepared to increase the specific surface area, improve the binding ability with water molecules and the loading amount of silver ions, and improve the skin-friendly and antibacterial properties of the soft and skin-friendly fabrics; formaldehyde-modified bamboo cellulose is polymerized and deposited on the surface The natural ingredient bamboo fiber is introduced into the soft and skin-friendly fabric by using 2,6-pyridinedimethylamine, 2-vinyl-4,6-diamino-1,3,5-triazine, and the skin-friendly performance of the soft and skin-friendly fabric is improved. The stable five-membered ring structure of the chelated metal is constructed through the Schiff base reaction to chelate the free silver ions and further improve the antibacterial performance of the soft and skin-friendly fabric. At the same time, the triazine structure in 2-vinyl-4,6-diamino-1,3,5-triazine can generate non-flammable nitrogen-containing gas during combustion, which absorbs heat, dilutes the oxygen concentration, and improves the flame retardant performance of the soft and skin-friendly fabric.

[0019] Secondly, terephthalic acid, vinyl terephthalic acid, ethylene glycol and N-methyldiethanolamine are polymerized to obtain pre-modified polyester powder; the pre-modified polyester powder and 4-(bromomethyl)-2,6-di-tert-butylphenol are reacted to obtain modified polyester; the modified polyester, modified silica microspheres and hydrogen-containing silicone oil are mixed and electrospun to obtain soft and skin-friendly fabrics; tertiary amine structure and carbon-carbon double bond structure are introduced into the polyester main chain by polymerization, and reacted with 4-(bromomethyl)-2,6-di-tert-butylphenol, and the grafted hindered phenol structure can capture and neutralize free radicals, thereby improving the anti-aging properties of the soft and skin-friendly fabric; at the same time, the quaternary ammonium salt structure is formed to improve the antistatic properties of the soft and skin-friendly fabric; through the hydrosilylation reaction, hydrogen-containing silicone oil is used to form a cross-linked network between the modified polyester and the modified silica microspheres, and at the same time, the silicon-oxygen flexible chain segment is increased to improve the mechanical properties and softness of the soft and skin-friendly fabric. DETAILED DESCRIPTION

[0020] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention. Example 1

[0021] A method for preparing a soft and skin-friendly fabric, the method for preparing the soft and skin-friendly fabric comprising the following preparation steps: (1) 0.07 mol / L silver nitrate aqueous solution and template dispersion were mixed in a volume ratio of 1:0.5, stirred at 20°C and 100 rpm for 65 min, 0.07 g / L polyvinyl pyrrolidone alcohol solution (0.3 times the volume of the silver nitrate aqueous solution) was added, stirring was continued for 3 h, ammonia (0.05 times the volume of the silver nitrate aqueous solution) was added, stirring was continued at 200 rpm for 65 min, 0.01 times the volume of the silver nitrate aqueous solution of tetraethyl orthosilicate was added at a uniform rate within 20 min, stirring was continued for 3 h, filtered, washed with deionized water for 3 times, dried at 55°C for 12 h, heated to 600°C at a rate of 0.5°C / min and kept warm for 5 h, and naturally cooled to room temperature to obtain silver-loaded porous silica microspheres; (2) The formaldehyde-modified bamboo cellulose, silver-loaded porous silica microspheres and N,N-dimethylformamide were mixed in a mass ratio of 1:2:199, stirred at 20°C and 200 rpm for 30 min, 2,6-pyridinedimethylamine (0.4 times the molar amount of aldehyde group in the formaldehyde-modified bamboo cellulose) and 2-vinyl-4,6-diamino-1,3,5-triazine (0.4 times the molar amount of aldehyde group in the formaldehyde-modified bamboo cellulose) were added, the temperature was raised to 75°C and stirring was continued for 4 h, the mixture was naturally cooled to room temperature and filtered, washed with deionized water for 3 times, and dried at 65°C for 12 h to obtain modified porous silica microspheres; (3) Terephthalic acid, vinyl terephthalic acid, ethylene glycol, N-methyldiethanolamine and antimony acetate were mixed in a mass ratio of 1:0.3:1.3:0.3:0.01, stirred for 5 h in a nitrogen atmosphere at 210°C, 400 rpm and 0.02 MPa, the pressure was reduced to 50 Pa and the stirring was continued for 20 min, the temperature was increased to 255°C and 45 Pa and the reaction was continued for 2 h, poured into deionized water, cooled and pelletized, ground and sieved through 80 mesh to obtain pre-modified polyester powder; pre-modified polyester powder, 4-(bromomethyl)-2,6-di-tert-butylphenol and dichloromethane were mixed in a mass ratio of 1:0.5:19, stirred for 7 h in a nitrogen environment at 75°C and 200 rpm, naturally cooled to room temperature and filtered, washed with saturated salt water and deionized water for 3 times respectively, and dried at 55°C for 10 h to obtain modified polyester; (4) The modified polyester, modified silica microspheres, hydrogenated silicone oil, trifluoroacetic acid and dichloromethane were mixed in a mass ratio of 1:0.15:1:4.3:0.9, stirred at 20°C and 200 rpm for 5 h, 0.01 times the mass of the modified polyester was added with chloroplatinic acid, and the stirring was continued for 20 min. The mixture was allowed to stand for 20 min, and electrospinning was performed under the conditions of a spinning voltage of 27 kV, a receiving distance of 14 cm, and a spinning solution push rate of 0.002 mm / s. After completion, the mixture was allowed to stand at 60°C for 8 h, washed with deionized water for 3 times, and dried at 55°C for 10 h to obtain spun fibers. The spun fibers were spun and woven by a textile machine to obtain soft and skin-friendly fabrics. Example 2

[0022] A method for preparing a soft and skin-friendly fabric, the method for preparing the soft and skin-friendly fabric comprising the following preparation steps: (1) 0.075 mol / L silver nitrate aqueous solution and template dispersion were mixed in a volume ratio of 1:1, stirred at 25°C and 150 rpm for 60 min, 0.075 g / L polyvinyl pyrrolidone alcohol solution (0.4 times the volume of the silver nitrate aqueous solution) was added, stirring was continued for 2 h, ammonia (0.06 times the volume of the silver nitrate aqueous solution) was added, stirring was continued at 250 rpm for 60 min, 0.02 times the volume of the silver nitrate aqueous solution of tetraethyl orthosilicate was added at a uniform rate within 25 min, stirring was continued for 2 h, filtered, washed with deionized water 4 times, dried at 60°C for 11 h, heated to 550°C at a rate of 1°C / min and kept warm for 6 h, and naturally cooled to room temperature to obtain silver-loaded porous silica microspheres; (2) The formaldehyde-modified bamboo cellulose, silver-loaded porous silica microspheres and N,N-dimethylformamide were mixed in a mass ratio of 1:2.5:200, stirred at 25°C and 250 rpm for 25 min, 2,6-pyridinedimethylamine (0.5 times the molar amount of aldehyde group in the formaldehyde-modified bamboo cellulose) and 2-vinyl-4,6-diamino-1,3,5-triazine (0.5 times the molar amount of aldehyde group in the formaldehyde-modified bamboo cellulose) were added, the temperature was raised to 80°C and stirring was continued for 3 h, the mixture was naturally cooled to room temperature and filtered, washed with deionized water for 4 times, and dried at 70°C for 11 h to obtain modified porous silica microspheres; (3) Terephthalic acid, vinyl terephthalic acid, ethylene glycol, N-methyldiethanolamine and antimony acetate were mixed in a mass ratio of 1:0.35:1.35:0.4:0.015, stirred for 4 hours at 215°C, 450rpm and 0.03MPa in a nitrogen atmosphere, reduced the pressure to 75Pa and continued stirring for 15min, heated to 260°C and 50Pa and continued reacting for 1.5h, poured into deionized water, cooled and pelletized, ground and sieved through 90 mesh to obtain pre-modified polyester powder; pre-modified polyester powder, 4-(bromomethyl)-2,6-di-tert-butylphenol and dichloromethane were mixed in a mass ratio of 1:0.55:20, stirred for 6 hours at 80°C and 250rpm in a nitrogen environment, naturally cooled to room temperature and filtered, washed with saturated salt water and deionized water for 4 times respectively, and dried at 60°C for 9h to obtain modified polyester; (4) The modified polyester, modified silica microspheres, hydrogenated silicone oil, trifluoroacetic acid and dichloromethane were mixed in a mass ratio of 1:0.16:1.5:4.4:1.1, stirred at 25°C and 250 rpm for 4 h, 0.015 times the mass of the modified polyester was added with chloroplatinic acid, and the stirring was continued for 15 min. The mixture was allowed to stand for 15 min, and electrospinning was performed under the conditions of a spinning voltage of 28 kV, a receiving distance of 15 cm, and a spinning solution push rate of 0.003 mm / s. After completion, the mixture was allowed to stand at 65°C for 7 h, washed with deionized water 4 times, and dried at 60°C for 9 h to obtain spun fibers. The spun fibers were spun and woven by a textile machine to obtain soft and skin-friendly fabrics. Example 3

[0023] A method for preparing a soft and skin-friendly fabric, the method for preparing the soft and skin-friendly fabric comprising the following preparation steps: (1) 0.08 mol / L silver nitrate aqueous solution and template dispersion were mixed in a volume ratio of 1:1.5, stirred at 30°C and 200 rpm for 55 min, 0.08 g / L polyvinyl pyrrolidone alcohol solution (0.5 times the volume of the silver nitrate aqueous solution) was added, stirring was continued for 1 h, ammonia (0.07 times the volume of the silver nitrate aqueous solution) was added, stirring was continued at 300 rpm for 55 min, 0.03 times the volume of the silver nitrate aqueous solution of tetraethyl orthosilicate was added at a uniform rate within 30 min, stirring was continued for 1 h, and then filtered, washed with deionized water for 5 times, dried at 65°C for 10 h, heated to 500°C at a rate of 1.5°C / min and kept warm for 7 h, and naturally cooled to room temperature to obtain silver-loaded porous silica microspheres; (2) The formaldehyde-modified bamboo cellulose, silver-loaded porous silica microspheres and N,N-dimethylformamide were mixed in a mass ratio of 1:3:201, stirred at 30°C and 300 rpm for 20 min, 2,6-pyridinedimethylamine (0.6 times the molar amount of aldehyde group in the formaldehyde-modified bamboo cellulose) and 2-vinyl-4,6-diamino-1,3,5-triazine (0.6 times the molar amount of aldehyde group in the formaldehyde-modified bamboo cellulose) were added, the temperature was raised to 85°C and stirring was continued for 2 h, the mixture was naturally cooled to room temperature and filtered, washed with deionized water for 5 times, and dried at 75°C for 10 h to obtain modified porous silica microspheres; (3) Terephthalic acid, vinyl terephthalic acid, ethylene glycol, N-methyldiethanolamine and antimony acetate were mixed in a mass ratio of 1:0.4:1.4:0.5:0.02, stirred for 3 h in a nitrogen atmosphere at 220°C, 500 rpm and 0.04 MPa, reduced the pressure to 100 Pa and continued stirring for 10 min, heated to 265°C and 55 Pa and continued reacting for 1 h, poured into deionized water, cooled and taken out, cut into pellets, ground and sieved through 100 mesh to obtain pre-modified polyester powder; pre-modified polyester powder, 4-(bromomethyl)-2,6-di-tert-butylphenol and dichloromethane were mixed in a mass ratio of 1:0.6:21, stirred for 5 h in a nitrogen environment at 85°C and 300 rpm, naturally cooled to room temperature and filtered, washed with saturated salt water and deionized water for 5 times respectively, and dried at 65°C for 8 h to obtain modified polyester; (4) The modified polyester, modified silica microspheres, hydrogenated silicone oil, trifluoroacetic acid and dichloromethane were mixed in a mass ratio of 1:0.17:2:4.5:1.3, stirred at 30°C and 300 rpm for 3 h, 0.02 times the mass of modified polyester chloroplatinic acid was added, stirring was continued for 10 min, and the mixture was allowed to stand for 10 min. Electrospinning was performed under the conditions of spinning voltage 29 kV, receiving distance 16 cm, and spinning solution push rate 0.004 mm / s. After completion, the mixture was allowed to stand at 70°C for 6 h, washed with deionized water 5 times, and dried at 65°C for 8 h to obtain spun fibers. The spun fibers were spun and woven by a textile machine to obtain soft and skin-friendly fabrics.

[0024] Comparative Example 1 A method for preparing a soft and skin-friendly fabric, the method for preparing the soft and skin-friendly fabric comprising the following preparation steps: (1) 0.075 mol / L silver nitrate aqueous solution and template dispersion were mixed in a volume ratio of 1:1, stirred at 25°C and 150 rpm for 60 min, 0.075 g / L polyvinyl pyrrolidone alcohol solution (0.4 times the volume of the silver nitrate aqueous solution) was added, stirring was continued for 2 h, ammonia (0.06 times the volume of the silver nitrate aqueous solution) was added, stirring was continued at 250 rpm for 60 min, 0.02 times the volume of the silver nitrate aqueous solution of tetraethyl orthosilicate was added at a uniform rate within 25 min, stirring was continued for 2 h, filtered, washed with deionized water 4 times, dried at 60°C for 11 h, heated to 550°C at a rate of 1°C / min and kept warm for 6 h, and naturally cooled to room temperature to obtain silver-loaded porous silica microspheres; (2) Terephthalic acid, vinyl terephthalic acid, ethylene glycol, N-methyldiethanolamine and antimony acetate were mixed in a mass ratio of 1:0.35:1.35:0.4:0.015, stirred for 4 hours at 215°C, 450rpm and 0.03MPa in a nitrogen atmosphere, reduced the pressure to 75Pa and continued to stir for 15min, heated to 260°C and 50Pa and continued to react for 1.5h, poured into deionized water, cooled and pelletized, ground and sieved through 90 mesh to obtain pre-modified polyester powder; pre-modified polyester powder, 4-(bromomethyl)-2,6-di-tert-butylphenol and dichloromethane were mixed in a mass ratio of 1:0.55:20, stirred for 6 hours at 80°C and 250rpm in a nitrogen environment, naturally cooled to room temperature and filtered, washed with saturated salt water and deionized water for 4 times respectively, and dried at 60°C for 9h to obtain modified polyester; (3) The modified polyester, silver-loaded porous silica microspheres, hydrogenated silicone oil, trifluoroacetic acid and dichloromethane were mixed in a mass ratio of 1:0.16:1.5:4.4:1.1, stirred at 25°C and 250 rpm for 4 h, 0.015 times the mass of the modified polyester chloroplatinic acid was added, stirring was continued for 15 min, and the mixture was allowed to stand for 15 min. Electrospinning was performed under the conditions of a spinning voltage of 28 kV, a receiving distance of 15 cm, and a spinning solution push rate of 0.003 mm / s. After completion, the mixture was allowed to stand at 65°C for 7 h, washed with deionized water 4 times, and dried at 60°C for 9 h to obtain spun fibers. The spun fibers were spun and woven on a textile machine to obtain soft and skin-friendly fabrics.

[0025] Comparative Example 2 A method for preparing a soft and skin-friendly fabric, the method for preparing the soft and skin-friendly fabric comprising the following preparation steps: (1) 0.075 mol / L silver nitrate aqueous solution and template dispersion were mixed in a volume ratio of 1:1, stirred at 25°C and 150 rpm for 60 min, 0.075 g / L polyvinyl pyrrolidone alcohol solution (0.4 times the volume of the silver nitrate aqueous solution) was added, stirring was continued for 2 h, ammonia (0.06 times the volume of the silver nitrate aqueous solution) was added, stirring was continued at 250 rpm for 60 min, 0.02 times the volume of the silver nitrate aqueous solution of tetraethyl orthosilicate was added at a uniform rate within 25 min, stirring was continued for 2 h, filtered, washed with deionized water 4 times, dried at 60°C for 11 h, heated to 550°C at a rate of 1°C / min and kept warm for 6 h, and naturally cooled to room temperature to obtain silver-loaded porous silica microspheres; (2) The formaldehyde-modified bamboo cellulose, silver-loaded porous silica microspheres and N,N-dimethylformamide were mixed in a mass ratio of 1:2.5:200, stirred at 25°C and 250 rpm for 25 min, 2,6-pyridinedimethylamine (0.5 times the molar amount of aldehyde group in the formaldehyde-modified bamboo cellulose) and 2-vinyl-4,6-diamino-1,3,5-triazine (0.5 times the molar amount of aldehyde group in the formaldehyde-modified bamboo cellulose) were added, the temperature was raised to 80°C and stirring was continued for 3 h, the mixture was naturally cooled to room temperature and filtered, washed with deionized water for 4 times, and dried at 70°C for 11 h to obtain modified porous silica microspheres; (3) Terephthalic acid, vinyl terephthalic acid, ethylene glycol, N-methyldiethanolamine and antimony acetate were mixed in a mass ratio of 1:0.35:1.35:0.4:0.015, stirred for 4 h in a nitrogen atmosphere at 215°C, 450 rpm and 0.03 MPa, reduced the pressure to 75 Pa and continued stirring for 15 min, heated to 260°C and 50 Pa and continued to react for 1.5 h, poured into deionized water, cooled, taken out and pelletized, ground and sieved through 90 mesh to obtain modified polyester; (4) The modified polyester, modified silica microspheres, hydrogenated silicone oil, trifluoroacetic acid and dichloromethane were mixed in a mass ratio of 1:0.16:1.5:4.4:1.1, stirred at 25°C and 250 rpm for 4 h, 0.015 times the mass of the modified polyester was added with chloroplatinic acid, and the stirring was continued for 15 min. The mixture was allowed to stand for 15 min, and electrospinning was performed under the conditions of a spinning voltage of 28 kV, a receiving distance of 15 cm, and a spinning solution push rate of 0.003 mm / s. After completion, the mixture was allowed to stand at 65°C for 7 h, washed with deionized water 4 times, and dried at 60°C for 9 h to obtain spun fibers. The spun fibers were spun and woven by a textile machine to obtain soft and skin-friendly fabrics.

[0026] Comparative Example 3 A method for preparing a soft and skin-friendly fabric, the method for preparing the soft and skin-friendly fabric comprising the following preparation steps: (1) 0.075 mol / L silver nitrate aqueous solution and template dispersion were mixed in a volume ratio of 1:1, stirred at 25°C and 150 rpm for 60 min, 0.075 g / L polyvinyl pyrrolidone alcohol solution (0.4 times the volume of the silver nitrate aqueous solution) was added, stirring was continued for 2 h, ammonia (0.06 times the volume of the silver nitrate aqueous solution) was added, stirring was continued at 250 rpm for 60 min, 0.02 times the volume of the silver nitrate aqueous solution of tetraethyl orthosilicate was added at a uniform rate within 25 min, stirring was continued for 2 h, filtered, washed with deionized water 4 times, dried at 60°C for 11 h, heated to 550°C at a rate of 1°C / min and kept warm for 6 h, and naturally cooled to room temperature to obtain silver-loaded porous silica microspheres; (2) The formaldehyde-modified bamboo cellulose, silver-loaded porous silica microspheres and N,N-dimethylformamide were mixed in a mass ratio of 1:2.5:200, stirred at 25°C and 250 rpm for 25 min, 2,6-pyridinedimethylamine (0.5 times the molar amount of aldehyde group in the formaldehyde-modified bamboo cellulose) and 2-vinyl-4,6-diamino-1,3,5-triazine (0.5 times the molar amount of aldehyde group in the formaldehyde-modified bamboo cellulose) were added, the temperature was raised to 80°C and stirring was continued for 3 h, the mixture was naturally cooled to room temperature and filtered, washed with deionized water for 4 times, and dried at 70°C for 11 h to obtain modified porous silica microspheres; (3) Terephthalic acid, ethylene glycol, N-methyldiethanolamine and antimony acetate were mixed in a mass ratio of 1:1.35:0.4:0.015, stirred at 215°C, 450rpm and 0.03MPa for 4h in a nitrogen atmosphere, reduced the pressure to 75Pa and continued stirring for 15min, heated to 260°C and 50Pa and continued reacting for 1.5h, poured into deionized water, cooled and taken out, cut into pellets, ground and sieved through 90 mesh to obtain pre-modified polyester powder; pre-modified polyester powder, 4-(bromomethyl)-2,6-di-tert-butylphenol and dichloromethane were mixed in a mass ratio of 1:0.55:20, stirred at 80°C and 250rpm for 6h in a nitrogen environment, naturally cooled to room temperature and filtered, washed with saturated salt water and deionized water for 4 times respectively, and dried at 60°C for 9h to obtain modified polyester; (4) The modified polyester, modified silica microspheres, hydrogenated silicone oil, trifluoroacetic acid and dichloromethane were mixed in a mass ratio of 1:0.16:1.5:4.4:1.1, stirred at 25°C and 250 rpm for 4 h, 0.015 times the mass of the modified polyester was added with chloroplatinic acid, and the stirring was continued for 15 min. The mixture was allowed to stand for 15 min, and electrospinning was performed under the conditions of a spinning voltage of 28 kV, a receiving distance of 15 cm, and a spinning solution push rate of 0.003 mm / s. After completion, the mixture was allowed to stand at 65°C for 7 h, washed with deionized water 4 times, and dried at 60°C for 9 h to obtain spun fibers. The spun fibers were spun and woven by a textile machine to obtain soft and skin-friendly fabrics.

[0027] Test Example 1 1. Skin-friendly Test method: The soft and skin-friendly fabrics obtained in each embodiment and the comparative example are weighed with a GB204 electronic analytical balance according to GB / T21655, and the sample mass m0 is soaked in deionized water at 20°C and humidity 65% ​​for 5 minutes, then taken out and hung vertically for 10 seconds without dripping, and the sample mass m1 is weighed, and the water absorption rate = m1-m0 / m0*100% is calculated.

[0028] 2. Flexibility Test method: The soft and skin-friendly fabrics obtained in each embodiment and the comparative example are taken in size of 25cm×2.5cm according to GB / T18318, and the longitudinal bending length is measured by LLY-01 electronic stiffness meter and intelligent style meter.

[0029] 3. Antibacterial Test method: Take two test samples of the soft and skin-friendly fabrics obtained in each embodiment and the comparative example according to GB / T20944, and take one sample to test the antibacterial rate R1 against Staphylococcus aureus; the other sample is washed in deionized water at 200rpm for 30s, dried at 25°C for 8h, and washed and dried repeatedly 10 times, and the antibacterial rate R2 against Staphylococcus aureus is tested again, and the antibacterial retention rate R2 / R1*100% is calculated to judge the persistent antibacterial property.

[0030] Table 1 below shows the analysis results of the softness, skin affinity and antibacterial properties of the soft and skin-friendly fabrics of Examples 1 to 3 of the present invention and Comparative Examples 1 to 3.

[0031] Table 1

[0032] From the comparison of the experimental data of Examples 1 to 3 and Comparative Examples 1 to 3 in Table 1, it can be found that the soft and skin-friendly fabric prepared by the present invention has good softness, skin-friendliness and antibacterial properties.

[0033] By comparison, the bending lengths of Examples 1, 2, and 3 compared with the comparative example illustrate that the soft, skin-friendly fabrics prepared by the present invention all have good softness.

[0034] By comparison, Examples 1, 2, and 3 have higher water absorption and antibacterial retention rates than Comparative Example 1, indicating that formaldehyde-modified bamboo cellulose, 2,6-pyridinedimethylamine, and 2-vinyl-4,6-diamino-1,3,5-triazine are polymerized and deposited on the surface of silver-loaded porous silica microspheres, and natural bamboo fiber is introduced to improve the skin-friendly properties of soft and skin-friendly fabrics; a stable five-membered ring structure of chelated metal is constructed through Schiff base reaction to chelate free silver ions and improve the long-lasting antibacterial properties of soft and skin-friendly fabrics.

[0035] Test Example 2 1. Antistatic Test method: The soft and skin-friendly fabrics obtained in each embodiment and the comparative example were tested for the static voltage half-life in a size of 6cm×8cm according to GB / T12703.

[0036] 2. Flame retardancy Test method: The soft and skin-friendly fabrics obtained in each embodiment and the comparative example were tested for limiting oxygen index according to GB / T8746.

[0037] 3. Mechanical properties Test method: The spun fibers obtained in each example and the comparative example were tested for breaking strength σ0 at a tensile rate of 100 mm / min using a YGO26PC-500 electronic textile strength tester according to GB / T3916.

[0038] 4. Anti-aging Test method: The soft and skin-friendly fabrics obtained in each embodiment and the comparative example were placed in a blackboard temperature of 65°C, a box humidity of 50%, and a light intensity of 550W / m 2 , treat for 48 hours under the condition of 18min spray cycle, test the breaking strength σ1 again according to GB / T3916, and calculate the strength retention rate σ1 / σ0*100%.

[0039] Table 2 below shows the analysis results of the antistatic, flame retardant, aging resistance and mechanical properties of the soft and skin-friendly fabrics of Examples 1 to 3 of the present invention and Comparative Examples 1 to 3.

[0040] Table 2

[0041] From the comparison of the experimental data of Examples 1 to 3 and Comparative Examples 1 to 3 in Table 2, it can be found that the soft and skin-friendly fabric prepared by the present invention has good antistatic properties, flame retardancy, aging resistance and mechanical properties.

[0042] By comparison, the limiting oxygen index and breaking strength of Examples 1, 2, and 3 are higher than those of Comparative Example 1, indicating that the triazine structure introduced by polymerizing and depositing formaldehyde-modified bamboo cellulose, 2,6-pyridinedimethylamine, and 2-vinyl-4,6-diamino-1,3,5-triazine on the surface of silver-loaded porous silica microspheres can generate non-flammable nitrogen-containing gas during combustion, absorb heat, dilute oxygen concentration, and improve the flame retardant properties of soft and skin-friendly fabrics; at the same time, the retained carbon-carbon double bonds can be grafted with hydrogenated silicone oil through a silylation reaction to form a cross-linked network, thereby improving the mechanical properties of soft and skin-friendly fabrics.

[0043] By comparison, the electrostatic voltage half-life of Examples 1, 2, and 3 is short and the strength retention rate is high compared with that of Comparative Example 2, which indicates that a tertiary amine structure and a carbon-carbon double bond structure are introduced into the polyester main chain through polymerization, and react with 4-(bromomethyl)-2,6-di-tert-butylphenol. The grafted hindered phenol structure can capture and neutralize free radicals, thereby improving the anti-aging properties of the soft and skin-friendly fabric; at the same time, the quaternary ammonium salt structure formed improves the antistatic properties of the soft and skin-friendly fabric.

[0044] By comparison, the breaking strength of Examples 1, 2, and 3 is higher than that of Comparative Example 3, which indicates that a cross-linked network is formed between the modified polyester and the modified silica microspheres by the hydrogenated silicone oil through the hydrosilylation reaction, thereby improving the mechanical properties of the soft and skin-friendly fabric.

[0045] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations within the meaning and scope of the equivalent elements of the claims be included in the invention. Any marking in a claim should not be considered as limiting the claim to which it relates.

Claims

1. A soft and skin-friendly fabric, characterized in that: The soft and skin-friendly fabric is obtained by electrostatic spinning of modified polyester, modified silica microspheres and hydrogen-containing silicone oil; The modified polyester is obtained by polymerizing terephthalic acid, vinyl terephthalic acid, ethylene glycol and N-methyldiethanolamine and then reacting with 4-(bromomethyl)-2,6-di-tert-butylphenol; The modified silica microspheres are obtained by loading silver ions onto tetraethyl orthosilicate and then polymerizing and depositing aldehyde-modified bamboo cellulose, 2,6-pyridinedimethylamine and 2-vinyl-4,6-diamino-1,3,5-triazine on the surface.

2. A method for preparing a soft and skin-friendly fabric, characterized in that: The method comprises the following preparation steps: (1) Mix 0.07~0.08 mol / L silver nitrate aqueous solution and template dispersion in a volume ratio of 1:(0.5~1.5), stir at 20~30℃ and 100~200 rpm for 55~65 min, add 0.3~0.5 times the volume of silver nitrate aqueous solution and 0.07~0.08 g / L polyvinyl pyrrolidone alcohol solution, continue stirring for 1~3 h, add 0.05~0.07 times the volume of silver nitrate aqueous solution and ammonia water. Stirring at 200-300 rpm for 55-65 min, adding 0.01-0.03 times the volume of the silver nitrate aqueous solution of tetraethyl orthosilicate at a uniform rate within 20-30 min, continuing stirring for 1-3 h and filtering, washing with deionized water 3-5 times, drying at 55-65° C. for 10-12 h, heating to 500-600° C. at a rate of 0.5-1.5° C. / min and keeping the temperature for 5-7 h, and naturally cooling to room temperature to obtain silver-loaded porous silica microspheres; (2) The formaldehyde-modified bamboo cellulose, silver-loaded porous silica microspheres and N,N-dimethylformamide were mixed in a mass ratio of 1:(2-3):(199-201), stirred at 20-30°C and 200-300 rpm for 20-30 min, 2,6-pyridinedimethylamine with a molar amount of 0.4-0.6 times the aldehyde group in the formaldehyde-modified bamboo cellulose and 2-vinyl-4,6-diamino-1,3,5-triazine with a molar amount of 0.4-0.6 times the aldehyde group in the formaldehyde-modified bamboo cellulose were added, the temperature was raised to 75-85°C and stirring was continued for 2-4 h, the mixture was naturally cooled to room temperature and filtered, washed with deionized water for 3-5 times, and dried at 65-75°C for 10-12 h to obtain modified porous silica microspheres; (3) Mix terephthalic acid, vinyl terephthalic acid, ethylene glycol, N-methyldiethanolamine and antimony acetate in a mass ratio of 1:(1.1~1.2):(0.3~0.4):(0.01~0.02), stir for 3~5 hours in a nitrogen atmosphere at 210~220℃, 400~500rpm, and 0.02~0.04MPa, reduce the pressure to 50~100Pa and continue stirring for 10~20min, increase the temperature to 255~265℃, 45~55Pa and continue the reaction for 1~2h, then pour in deionized water, and after cooling, the pellets are taken out and sieved through 80-100 meshes to obtain pre-modified polyester powder; the pre-modified polyester powder, 4-(bromomethyl)-2,6-di-tert-butylphenol and dichloromethane are mixed in a mass ratio of 1:(0.5-0.6):(19-21), stirred at 75-85°C and 200-300rpm for 5-7h under a nitrogen environment, naturally cooled to room temperature and then filtered, washed with saturated salt water and deionized water for 3-5 times respectively, and dried at 55-65°C for 8-10h to obtain modified polyester; (4) Mix terephthalic acid, vinyl terephthalic acid, ethylene glycol, N-methyldiethanolamine and antimony acetate in a mass ratio of 1:(0.3~0.4):(1.3~1.4):(0.3~0.5):(0.01~0.02), stir at 200~300 rpm for 3~5 hours at 20~30°C, add 0.01~0.02 times the mass of modified polyester chloroplatinic acid, and continue stirring for 10~20 minutes. , let it stand for 10~20min, carry out electrostatic spinning under the conditions of spinning voltage 27~29kV, receiving distance 14~16cm, spinning solution push rate 0.002~0.004mm / s, let it stand at 60~70℃ for 6~8h, wash with deionized water 3~5 times, and dry at 55~65℃ for 8~10h to obtain spun fibers; the spun fibers are spun and woven by a textile machine to obtain soft and skin-friendly fabrics.

3. The method for preparing a soft and skin-friendly fabric according to claim 2, characterized in that: The template dispersion in step (1) is prepared by mixing polystyrene microsphere powder and sulfuric acid solution with a mass fraction of 70-80% in a mass ratio of 1:(33-34), ultrasonically dispersing at 35-45° C. for 40-50 min, naturally cooling to room temperature and centrifuging, washing with anhydrous ethanol for 3-5 times, adding anhydrous ethanol with a mass fraction of 95-105 times that of the polystyrene microsphere powder, and stirring at 20-30° C. and 200-300 rpm for 1-2 h.

4. The method for preparing a soft and skin-friendly fabric according to claim 2, characterized in that: The aldehyde-modified bamboo cellulose in step (2) is prepared by mixing bamboo fiber powder, sodium periodate and deionized water in a mass ratio of 1:(3-5):(3-5), adjusting the pH value to 3-5 with a hydrochloric acid solution having a mass fraction of 16-18%, stirring for 28-32 hours at 20-30° C. and 150-250 r / min under light-proof conditions, adding ethylene glycol in an amount of 1.4-1.6 times the mass of the bamboo fiber powder, continuing to stir for 1-2 hours, filtering, washing with deionized water for 3-5 times, and drying at 45-55° C. for 23-25 ​​hours.

5. The method for preparing a soft and skin-friendly fabric according to claim 2, characterized in that: The reaction equation for the aldehyde-modified bamboo cellulose in step (2) is: 。 6. The method for preparing a soft, skin-friendly fabric according to claim 2, characterized in that: The reaction equation for modifying the porous silica microspheres in step (2) is: 。 7. The method for preparing a soft, skin-friendly fabric according to claim 2, characterized in that: The reaction equation of the pre-modified polyester in step (3) is: ; Where R1 is: or .

8. The method for preparing a soft and skin-friendly fabric according to claim 2, characterized in that: The reaction equation for the modified polyester in step (3) is: ; Where R1 is: or .

Citation Information

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