High-sunscreen high-breath moisture-absorption quick-drying creased fabric and preparation method thereof
By blending modified carboxylated carbon nanotubes with matte PET chips and treating them with a complex cross-linking network, the problems of easy shedding and poor breathability of traditional sunscreen fabrics have been solved, achieving highly efficient flame retardant, antibacterial, and moisture-wicking quick-drying effects, thus improving the overall performance of the fabric.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- WUXI CENTURY WIND FASHION CO LTD
- Filing Date
- 2025-07-30
- Publication Date
- 2026-05-15
AI Technical Summary
Traditional sun protection fabrics suffer from issues such as UV protection additives easily detaching and affecting breathability. Polyester fabrics also have poor flame retardancy and antibacterial properties, and cannot absorb moisture and dry quickly in hot weather, making it difficult to meet consumers' multifunctional needs.
Modified polyester fibers were prepared by melt spinning modified carboxylated carbon nanotubes and matte PET chips. The base fabric was woven using a double-sided knitting machine and treated with a dialdehyde carboxymethyl chitosan solution. Then, a complex cross-linking network was constructed by combining gelatin and polyether epoxy co-modified silicone oil emulsion finishing agent to improve the flame retardancy, antibacterial properties and breathability of the fabric.
A green and environmentally friendly fabric with strong sun protection, high breathability, moisture absorption and quick-drying properties has been developed. It also has flame retardant, antibacterial and antistatic properties, as well as good protection and comfort.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of fabric technology, specifically to a highly sun-protective, breathable, moisture-wicking, quick-drying wrinkle-resistant fabric and its preparation method. Background Technology
[0002] As people's living standards improve, the demand for textiles is moving towards diversification, fashion, and functionality. Multifunctional textiles that combine UV protection, comfort, and breathability have become the focus of industry research and development.
[0003] Traditional sun-protective fabrics often use coatings or blends of UV-protective additives to improve UV resistance. While these provide basic protection, they generally suffer from problems such as the additives easily detaching and affecting breathability, making them unsuitable for prolonged wear. Furthermore, traditional polyester fabrics have poor flame retardancy and antibacterial properties, and in hot summer weather, they cannot wick away moisture quickly enough, failing to meet the growing demands of consumers. Summary of the Invention
[0004] The purpose of this invention is to provide a highly sun-protective, breathable, moisture-wicking, quick-drying wrinkle-resistant fabric and its preparation method, so as to solve the problems in the prior art.
[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution:
[0006] A method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric includes the following steps:
[0007] S1: Modified carboxylated carbon nanotubes, antioxidants, and PET chips are dried, blended, melt-spun, cooled, and wound to obtain modified polyester fibers;
[0008] S2: A double-sided knitted base fabric is woven from modified polyester fiber using a double-sided knitting machine; the inner layer of the double-sided knitted base fabric is woven from modified polyester fiber; the outer layer of the double-sided knitted base fabric is formed by interlacing modified polyester fiber or nylon fiber.
[0009] S3: First, the double-sided knitted base fabric is subjected to two dips and two nips with a dialdehyde carboxymethyl chitosan solution, pre-drying and baking, then dyed with dye, soaped, washed with water and dried to obtain the pre-treated base fabric.
[0010] S4: A finishing solution was prepared using gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, modified carboxylated carbon nanotubes, and deionized water.
[0011] S5: The pre-treated base fabric is immersed in the finishing solution, padded, wrinkled, shaped, and dried to obtain a highly sun-resistant, breathable, moisture-wicking, and quick-drying wrinkled fabric.
[0012] Furthermore, the PET slices are either semi-dull PET slices or fully dull PET slices.
[0013] Furthermore, in the preparation of modified polyester fibers, the mass ratio of antioxidant, modified carboxylated carbon nanotubes, and PET chips is 0.1:1:99.
[0014] Furthermore, the working conditions for the wrinkling process are: temperature 180-200℃, pressure 5-15 kg / cm². 2 The time is 10-30 seconds, and the wrinkling direction is either longitudinal or transverse.
[0015] When the dye is black, the UPF value of the fabric is higher than 2000.
[0016] During the wrinkling process, the fabric is laid on a backing paper, and then covered with another layer of backing paper to form a sandwich structure. This prevents the fabric from directly contacting the mold, which could lead to excessively deep creases or damage, and also protects the gloss of the fabric surface.
[0017] Furthermore, the mass ratio of nylon fiber to modified polyester fiber in the surface layer is 4:6.
[0018] Furthermore, the basis weight of the double-knitted base fabric is 108-112 g / m². 2 .
[0019] Furthermore, the working conditions for the two-dip and two-roll treatment are as follows: immersion time is 60s, roll residue is 100%, pre-drying conditions are: holding at 78-82℃ for 4-6min; baking conditions are: holding at 120-130℃ for 2-4min; and dyeing conditions are: holding at 85-90℃ for 50-60min, liquor ratio is 1:(40-55), and pH is 5.5.
[0020] Furthermore, the working conditions for the dip-rolling process are: three dips and three rolls, with a dip time of 90-100 seconds and a roll residue of 80%.
[0021] Furthermore, in the finishing solution, the mass ratio of gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, and modified carboxylated carbon nanotubes is 3:0.5:12:1, and the ratio of dialdehyde carboxymethyl chitosan to deionized water is 1g:(40-50)mL.
[0022] Furthermore, the polyether epoxy co-modified silicone oil emulsion is a compound of polyether epoxy co-modified silicone oil, emulsifier, and deionized water in a mass ratio of 5:1:10.
[0023] Furthermore, the preparation of dialdehyde carboxymethyl chitosan includes the following steps:
[0024] Carboxymethyl chitosan and deionized water were mixed, sodium periodate was added, the pH was adjusted to 3.5, and the mixture was stirred at 38-42℃ in the dark for 3-4 hours. Ethylene glycol was added, and the mixture was stirred at 18-25℃ for 20-30 minutes. The mixture was washed 3-5 times by centrifugation with tert-butanol, freeze-dried, and ground to obtain dialdehyde carboxymethyl chitosan.
[0025] Furthermore, the preparation of modified carboxylated carbon nanotubes includes the following steps:
[0026] (1) Mix zinc acetate dihydrate and methanol, add carboxylated carbon nanotubes and polyvinylpyrrolidone, sonicate for 8-10 min, heat to 58-60℃, add potassium hydroxide and methanol mixture, stir for 1-2 h, transfer to reaction vessel, keep at 178-180℃ for 11-12 h, filter, wash and dry to obtain composite carboxylated carbon nanotubes;
[0027] (2) Under a nitrogen atmosphere, the composite carboxylated carbon nanotubes, thionyl chloride, and N,N-dimethylformamide were mixed and stirred at 68-72℃ for 22-24h. The mixture was then dried under reduced pressure and transferred to N,N-dimethylformamide. The mixture was then heated to 58-62℃ and ultrasonically dispersed for 25-30min. A mixed solution of pyridine, N,N-dimethylformamide, and hyperbranched polyamide was added and stirred at 18-25℃ for 22-24h. The mixture was then filtered, washed until neutral, dried, and ground to obtain the multi-amino modified composite carboxylated carbon nanotubes.
[0028] (3) Mix polyamino-modified composite carboxylated carbon nanotubes, epoxy POSS containing DOPO, triethanolamine, and N,N-dimethylformamide, ultrasonically stir for 10-20 min, keep warm at 60-70℃ for 3-5 h, wash, and dry to obtain modified carboxylated carbon nanotubes.
[0029] Furthermore, the preparation of DOPO-containing epoxy-based POSS includes the following steps:
[0030] 1) Mix tetramethylammonium hydroxide pentahydrate, isopropanol, and deionized water, add a mixture of γ-(2,3-epoxypropoxy)propyltrimethoxysilane and isopropanol, stir at 28-32℃ for 6 hours, rotary evaporate, add toluene, heat to 88-90℃ and keep warm for 3-4 hours to obtain polyepoxy group POSS;
[0031] 2) Mix polyepoxy group POSS, DOPO, triphenylphosphine and toluene, heat to 118-120℃ and hold for 110-130 min, then distill under reduced pressure and dry to obtain epoxy group POSS containing DOPO.
[0032] Compared with the prior art, the beneficial effects of the present invention are:
[0033] This invention provides a highly sun-protective, breathable, moisture-wicking, and quick-drying wrinkle fabric and its preparation method. Through process and component design, a green, environmentally friendly, flame-retardant, antibacterial, and antistatic highly sun-protective, breathable, moisture-wicking, and quick-drying wrinkle fabric is prepared.
[0034] To improve the mechanical strength and antistatic properties of matte or semi-matte polyester fibers, carboxylated carbon nanotubes were blended with matte or semi-matte PET chips and melt-spun to prepare matte or semi-matte polyester fibers. To improve the UV resistance and antibacterial properties of polyester fibers, nano-zinc oxide composite carboxylated carbon nanotubes were prepared as composite nanoparticles using a solution method with carboxylated carbon nanotubes as the matrix. To improve the uniformity of the composite nanoparticles in polyester fibers, the composite nanoparticles were first subjected to acylation and then grafted with hyperbranched polyamide to obtain polyamine-modified composite carboxylated carbon nanotubes. To further improve the flame retardancy of polyester fibers, polyamine-modified composite carboxylated carbon nanotubes were grafted with DOPO-containing epoxy group POSS to obtain modified carboxylated carbon nanotubes.
[0035] The epoxy-based POSS containing DOPO was first prepared using γ-(2,3-epoxypropoxy)propyltrimethoxysilane as a raw material to obtain polyepoxy-based POSS, and then DOPO was grafted onto it to obtain POSS containing both DOPO and epoxy groups. This POSS was then grafted onto polyamino-modified composite carboxylated carbon nanotubes using an epoxy-amino reaction. Through the triple synergy of phosphorus, nitrogen, and silicon, highly efficient halogen-free flame retardancy was achieved. At the same time, the multiple active sites on the carboxylated carbon nanotubes were modified to improve the compatibility with polyester fiber matrix and achieve a long-lasting flame retardant and antibacterial effect.
[0036] Modified polyester fiber is used as raw material to weave a double-sided knitted base fabric using a double-sided knitting machine. The inner layer of the double-sided knitted base fabric is woven from modified polyester fiber. The outer layer of the double-sided knitted base fabric is formed by interlacing modified polyester fiber or nylon fiber. In order to improve the dye uptake rate of the base fabric, the base fabric is subjected to two dips and two nips with a dialdehyde carboxymethyl chitosan solution, pre-drying and baking, and then dyeing treatment, thereby achieving dyeing depth and improving dye fastness. Carboxymethyl chitosan is a water-soluble chitosan derivative, and the dialdehyde carboxymethyl chitosan is obtained by oxidizing carboxymethyl chitosan with sodium periodate.
[0037] To further improve the antibacterial, flame-retardant, UV-resistant, and moisture-wicking properties of the fabric, and to fix the dyed pre-treated base fabric, a finishing agent was prepared using gelatin, polyether-epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, modified carboxylated carbon nanotubes, and deionized water. This agent was then used to treat the pre-treated base fabric. By controlling the mass ratio of gelatin, polyether-epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, and modified carboxylated carbon nanotubes, a complex cross-linked network was constructed. Simultaneously, the modified carbon nanotubes, through multi-level pores, improved breathability and quick-drying properties. The introduction of the polyether-epoxy co-modified silicone oil emulsion maintained the fabric's soft touch, thus effectively balancing the needs for protection (flame retardancy, antibacterial, UV resistance, antistatic properties, etc.) and comfort.
[0038] The wrinkling process creates folds in the fabric, which reflect more ultraviolet rays, further enhancing the fabric's inherent UV protection and achieving a strong sun protection effect. At the same time, the wrinkling process gives the fabric an elegant luster, improving its aesthetic appeal. Detailed Implementation
[0039] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.
[0040] It should be noted that if the embodiments of the present invention involve directional indicators such as up, down, left, right, front, and back, these directional indicators are only used to explain the relative positional relationship and movement of components in a specific posture. If the specific posture changes, the directional indicators will also change accordingly. Furthermore, the technical solutions of the various embodiments can be combined with each other, but this must be based on the ability of those skilled in the art to implement them. When the combination of technical solutions is contradictory or cannot be implemented, it should be considered that such a combination of technical solutions does not exist and is not within the scope of protection claimed by the present invention.
[0041] The technical solution of the present invention will be further described in detail below with reference to specific embodiments. It should be understood that the following embodiments are only used to explain the present invention and are not intended to limit the present invention.
[0042] Example 1: A method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric, comprising the following steps:
[0043] S1: Modified carboxylated carbon nanotubes, antioxidants, and PET chips are dried, blended, melt-spun, cooled, and wound to obtain modified polyester fibers;
[0044] In the preparation of modified polyester fibers, the mass ratio of antioxidant, modified carboxylated carbon nanotubes, and PET chips is 0.1:1:99; the PET chips are semi-dull PET chips.
[0045] The working conditions for melt spinning are as follows: screw zone temperatures are 250℃, 270℃, and 280℃ respectively; spinning temperature is 280℃; draw ratio is 4; and winding speed is 600m / min.
[0046] The preparation of modified carboxylated carbon nanotubes includes the following steps:
[0047] (1) Mix 0.5g zinc acetate dihydrate and 30mL methanol, add 0.2g carboxylated carbon nanotubes and 0.1g polyvinylpyrrolidone, sonicate for 8min, heat to 58℃, add a mixture of 0.2g potassium hydroxide and 27mL methanol, stir for 1h, transfer to a reaction vessel, keep warm at 178℃ for 12h, filter, wash and dry to obtain composite carboxylated carbon nanotubes;
[0048] (2) Under a nitrogen atmosphere, 1g of composite carboxylated carbon nanotubes, 2mL of thionyl chloride and 20mL of N,N-dimethylformamide were mixed and stirred at 68℃ for 24h. The mixture was then dried under reduced pressure and transferred to 30mL of N,N-dimethylformamide. The mixture was then heated to 58℃ and ultrasonically dispersed for 30min. A mixed solution of 30mg of pyridine, 10mL of N,N-dimethylformamide and 0.5g of hyperbranched polyamide was added and stirred at 18℃ for 24h. The mixture was then filtered, washed until neutral, dried and ground to obtain multi-amino modified composite carboxylated carbon nanotubes.
[0049] (3) 1.5g of polyamino-modified composite carboxylated carbon nanotubes, 1.2g of epoxy POSS containing DOPO, 80mg of triethanolamine, and 5mL of N,N-dimethylformamide were mixed, ultrasonically stirred for 10min, kept at 60℃ for 5h, washed, and dried to obtain modified carboxylated carbon nanotubes.
[0050] The preparation of DOPO-containing epoxy-based POSS includes the following steps:
[0051] 1) Mix 1 mmol tetramethylammonium hydroxide pentahydrate, 5 mL isopropanol, and 90 mmol deionized water. Add a mixture of 30 mmol γ-(2,3-epoxypropoxy)propyltrimethoxysilane and 7 mL isopropanol. Stir at 28 °C for 6 h, evaporate by rotary evaporation, add 40 mL toluene, and heat to 88 °C for 4 h to obtain polyepoxy group POSS.
[0052] 2) Mix 50 mmol polyepoxy POSS, 200 mmol DOPO, 5 mmol triphenylphosphine and 50 mL toluene, heat to 118 °C and keep warm for 130 min, then distill under reduced pressure and dry to obtain epoxy POSS containing DOPO;
[0053] S2: A double-sided knitted base fabric is woven from modified polyester fiber using a double-sided knitting machine; the inner layer of the double-sided knitted base fabric is woven from modified polyester fiber; the outer layer of the double-sided knitted base fabric is formed by interlacing modified polyester fiber and nylon fiber.
[0054] The mass ratio of nylon fiber to modified polyester fiber in the surface layer is 4:6; the weight of the double-knitted base fabric is 110 g / m². 2 ;
[0055] S3: First, the double-sided knitted base fabric is subjected to two dips and two nips with a dialdehyde carboxymethyl chitosan solution, pre-drying and baking, then dyed with dye, soaped, washed with water and dried to obtain the pre-treated base fabric.
[0056] The preparation of the dialdehyde carboxymethyl chitosan solution includes the following steps: mixing dialdehyde carboxymethyl chitosan with a 2% acetic acid solution to prepare a 1% dialdehyde carboxymethyl chitosan solution.
[0057] S4: A finishing solution was prepared using gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, modified carboxylated carbon nanotubes, and deionized water.
[0058] In the finishing solution, the mass ratio of gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, and modified carboxylated carbon nanotubes is 3:0.5:12:1, and the volume ratio of dialdehyde carboxymethyl chitosan to deionized water is 1g:50mL.
[0059] The preparation of dialdehyde carboxymethyl chitosan includes the following steps:
[0060] Mix 5g of carboxymethyl chitosan with 100mL of deionized water, add 5g of sodium periodate, adjust the pH to 3.5, stir at 38℃ in the dark for 4h, add 1mL of ethylene glycol, stir at 18℃ for 30min, centrifuge and wash 3 times with tert-butanol, freeze dry and grind to obtain dialdehyde carboxymethyl chitosan.
[0061] The working conditions for the two-dip and two-nip treatment are: immersion time 60s, roll-off rate 100%, pre-drying conditions: holding at 78℃ for 6min, baking conditions: holding at 120℃ for 4min, and dyeing conditions: holding at 85℃ for 60min, liquor ratio 1:50, pH 5.5.
[0062] S5: The pre-treated base fabric is immersed in the finishing solution, then subjected to padding, wrinkling, shaping, and drying to obtain a strong sun protection, high breathability, moisture absorption and quick-drying wrinkled fabric.
[0063] The working conditions for the dip-rolling process are: three dips and three rolls, with a dip time of 90 seconds and a roll residue of 80%; the working conditions for the wrinkling process are: temperature 190℃ and pressure 10 kg / cm². 2 The time is 20 seconds, and the wrinkling direction is longitudinal.
[0064] Example 2: A method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric, comprising the following steps:
[0065] S1: Modified carboxylated carbon nanotubes, antioxidants, and PET chips are dried, blended, melt-spun, cooled, and wound to obtain modified polyester fibers;
[0066] In the preparation of modified polyester fibers, the mass ratio of antioxidant, modified carboxylated carbon nanotubes, and PET chips is 0.1:1:99; the PET chips are semi-dull PET chips.
[0067] The working conditions for melt spinning are as follows: screw zone temperatures are 250℃, 270℃, and 280℃ respectively; spinning temperature is 280℃; draw ratio is 4; and winding speed is 600m / min.
[0068] The preparation of modified carboxylated carbon nanotubes includes the following steps:
[0069] (1) Mix 0.5g zinc acetate dihydrate and 30mL methanol, add 0.2g carboxylated carbon nanotubes and 0.1g polyvinylpyrrolidone, sonicate for 9min, heat to 59℃, add a mixture of 0.2g potassium hydroxide and 27mL methanol, stir for 1.5h, transfer to a reaction vessel, keep warm at 179℃ for 11.5h, filter, wash and dry to obtain composite carboxylated carbon nanotubes;
[0070] (2) Under a nitrogen atmosphere, 1g of composite carboxylated carbon nanotubes, 2mL of thionyl chloride and 20mL of N,N-dimethylformamide were mixed and stirred at 70℃ for 23h. The mixture was then dried under reduced pressure and transferred to 30mL of N,N-dimethylformamide. The mixture was then heated to 60℃ and ultrasonically dispersed for 28min. A mixed solution of 30mg of pyridine, 10mL of N,N-dimethylformamide and 0.5g of hyperbranched polyamide was added and stirred at 20℃ for 23h. The mixture was then filtered, washed until neutral, dried and ground to obtain multi-amino modified composite carboxylated carbon nanotubes.
[0071] (3) 1.5g of polyamino-modified composite carboxylated carbon nanotubes, 1.2g of epoxy POSS containing DOPO, 80mg of triethanolamine, and 5mL of N,N-dimethylformamide were mixed, ultrasonically stirred for 15min, kept at 65℃ for 4h, washed, and dried to obtain modified carboxylated carbon nanotubes.
[0072] 1) Mix 1 mmol tetramethylammonium hydroxide pentahydrate, 5 mL isopropanol, and 90 mmol deionized water. Add a mixture of 30 mmol γ-(2,3-epoxypropoxy)propyltrimethoxysilane and 7 mL isopropanol. Stir at 30 °C for 6 h, evaporate by rotary evaporation, add 40 mL toluene, and heat to 89 °C for 3.5 h to obtain polyepoxy group POSS.
[0073] 2) The preparation of DOPO-containing epoxy POSS includes the following steps: 50 mmol of polyepoxy POSS, 200 mmol of DOPO, 5 mmol of triphenylphosphine and 50 mL of toluene are mixed, heated to 119 °C and kept at that temperature for 120 min, then distilled under reduced pressure and dried to obtain DOPO-containing epoxy POSS;
[0074] S2: A double-sided knitted base fabric is woven from modified polyester fiber using a double-sided knitting machine; the inner layer of the double-sided knitted base fabric is woven from modified polyester fiber; the outer layer of the double-sided knitted base fabric is formed by interlacing modified polyester fiber and nylon fiber.
[0075] The mass ratio of nylon fiber to modified polyester fiber in the surface layer is 4:6; the weight of the double-knitted base fabric is 110 g / m². 2 ;
[0076] S3: First, the double-sided knitted base fabric is subjected to two dips and two nips with a dialdehyde carboxymethyl chitosan solution, pre-drying and baking, then dyed with dye, soaped, washed with water and dried to obtain the pre-treated base fabric.
[0077] The preparation of the dialdehyde carboxymethyl chitosan solution includes the following steps: mixing dialdehyde carboxymethyl chitosan with a 2% acetic acid solution to prepare a 1% dialdehyde carboxymethyl chitosan solution.
[0078] S4: A finishing solution was prepared using gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, modified carboxylated carbon nanotubes, and deionized water.
[0079] In the finishing solution, the mass ratio of gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, and modified carboxylated carbon nanotubes is 3:0.5:12:1, and the volume ratio of dialdehyde carboxymethyl chitosan to deionized water is 1g:45mL.
[0080] The preparation of dialdehyde carboxymethyl chitosan includes the following steps:
[0081] Mix 5g of carboxymethyl chitosan with 100mL of deionized water, add 5g of sodium periodate, adjust the pH to 3.5, stir at 40℃ in the dark for 3.5h, add 1mL of ethylene glycol, stir at 20℃ for 25min, centrifuge and wash 4 times with tert-butanol, freeze dry and grind to obtain dialdehyde carboxymethyl chitosan.
[0082] The working conditions for the two-dip and two-nip treatment are: immersion time 60s, roll-off rate 100%, pre-drying conditions: holding at 80℃ for 5min, baking conditions: holding at 125℃ for 3min, and dyeing conditions: holding at 88℃ for 55min, liquor ratio 1:50, pH 5.5.
[0083] S5: The pre-treated base fabric is immersed in the finishing solution, then subjected to padding, wrinkling, shaping, and drying to obtain a strong sun protection, high breathability, moisture absorption and quick-drying wrinkled fabric.
[0084] The working conditions for the dip-rolling treatment are: three dips and three rolls, with a dip time of 95 seconds and a roll residue of 80%; the working conditions for the wrinkling treatment are: temperature 190℃ and pressure 10 kg / cm². 2 The time is 20 seconds, and the wrinkling direction is longitudinal.
[0085] Example 3: A method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric, comprising the following steps:
[0086] S1: Modified carboxylated carbon nanotubes, antioxidants, and PET chips are dried, blended, melt-spun, cooled, and wound to obtain modified polyester fibers;
[0087] In the preparation of modified polyester fibers, the mass ratio of antioxidant, modified carboxylated carbon nanotubes, and PET chips is 0.1:1:99; the PET chips are semi-dull PET chips.
[0088] The working conditions for melt spinning are as follows: screw zone temperatures are 250℃, 270℃, and 280℃ respectively; spinning temperature is 280℃; draw ratio is 4; and winding speed is 600m / min.
[0089] The preparation of modified carboxylated carbon nanotubes includes the following steps:
[0090] (1) Mix 0.5g zinc acetate dihydrate and 30mL methanol, add 0.2g carboxylated carbon nanotubes and 0.1g polyvinylpyrrolidone, sonicate for 10min, heat to 60℃, add a mixture of 0.2g potassium hydroxide and 27mL methanol, stir for 2h, transfer to a reaction vessel, keep warm at 180℃ for 11h, filter, wash and dry to obtain composite carboxylated carbon nanotubes;
[0091] (2) Under a nitrogen atmosphere, 1g of composite carboxylated carbon nanotubes, 2mL of thionyl chloride and 20mL of N,N-dimethylformamide were mixed and stirred at 72℃ for 22h. The mixture was then dried under reduced pressure and transferred to 30mL of N,N-dimethylformamide. The mixture was heated to 62℃ and ultrasonically dispersed for 25min. A mixed solution of 30mg of pyridine, 10mL of N,N-dimethylformamide and 0.5g of hyperbranched polyamide was added and stirred at 25℃ for 22h. The mixture was then filtered, washed until neutral, dried and ground to obtain multi-amino modified composite carboxylated carbon nanotubes.
[0092] (3) 1.5g of polyamino-modified composite carboxylated carbon nanotubes, 1.2g of epoxy POSS containing DOPO, 80mg of triethanolamine, and 5mL of N,N-dimethylformamide were mixed, ultrasonically stirred for 20min, kept at 70℃ for 3h, washed, and dried to obtain modified carboxylated carbon nanotubes.
[0093] The preparation of DOPO-containing epoxy-based POSS includes the following steps:
[0094] 1) Mix 1 mmol tetramethylammonium hydroxide pentahydrate, 5 mL isopropanol, and 90 mmol deionized water. Add a mixture of 30 mmol γ-(2,3-epoxypropoxy)propyltrimethoxysilane and 7 mL isopropanol. Stir at 32 °C for 6 h. Rotary evaporate the mixture. Add 40 mL toluene and heat to 90 °C for 3 h to obtain polyepoxy group POSS.
[0095] 2) Mix 50 mmol polyepoxy POSS, 200 mmol DOPO, 5 mmol triphenylphosphine and 50 mL toluene, heat to 120 °C and keep warm for 110 min, then distill under reduced pressure and dry to obtain epoxy POSS containing DOPO;
[0096] S2: A double-sided knitted base fabric is woven from modified polyester fiber using a double-sided knitting machine; the inner layer of the double-sided knitted base fabric is woven from modified polyester fiber; the outer layer of the double-sided knitted base fabric is formed by interlacing modified polyester fiber and nylon fiber.
[0097] The mass ratio of nylon fiber to modified polyester fiber in the surface layer is 4:6; the weight of the double-knitted base fabric is 110 g / m². 2 ;
[0098] S3: First, the double-sided knitted base fabric is subjected to two dips and two nips with a dialdehyde carboxymethyl chitosan solution, pre-drying and baking, then dyed with dye, soaped, washed with water and dried to obtain the pre-treated base fabric.
[0099] The preparation of the dialdehyde carboxymethyl chitosan solution includes the following steps: mixing dialdehyde carboxymethyl chitosan with a 2% acetic acid solution to prepare a 1% dialdehyde carboxymethyl chitosan solution.
[0100] S4: A finishing solution was prepared using gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, modified carboxylated carbon nanotubes, and deionized water.
[0101] In the finishing solution, the mass ratio of gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, and modified carboxylated carbon nanotubes is 3:0.5:12:1, and the volume ratio of dialdehyde carboxymethyl chitosan to deionized water is 1g:40mL.
[0102] The preparation of dialdehyde carboxymethyl chitosan includes the following steps:
[0103] Mix 5g of carboxymethyl chitosan with 100mL of deionized water, add 5g of sodium periodate, adjust the pH to 3.5, stir at 42℃ in the dark for 3h, add 1mL of ethylene glycol, stir at 25℃ for 20min, centrifuge and wash 5 times with tert-butanol, freeze dry and grind to obtain dialdehyde carboxymethyl chitosan.
[0104] The working conditions for the two-dip and two-nip treatment are: immersion time 60s, roll-off rate 100%, pre-drying conditions: holding at 82℃ for 4min; baking conditions: holding at 130℃ for 2min; and dyeing conditions: holding at 90℃ for 50min, liquor ratio 1:50, pH 5.5.
[0105] S5: The pre-treated base fabric is immersed in the finishing solution, then subjected to padding, wrinkling, shaping, and drying to obtain a strong sun protection, high breathability, moisture absorption and quick-drying wrinkled fabric.
[0106] The working conditions for the dip-rolling process are: three dips and three rolls, with a dip time of 100 seconds and a roll residue of 80%; the working conditions for the wrinkling process are: temperature 190℃ and pressure 10 kg / cm². 2 The time is 20 seconds, and the wrinkling direction is longitudinal.
[0107] Comparative Example 1: Using Example 3 as the control group, the modified carboxylated carbon nanotubes were replaced with composite carboxylated carbon nanotubes, while other processes were normal.
[0108] Comparative Example 2: With Example 3 as the control group, the mass ratio of gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, and modified carboxylated carbon nanotubes was 3:0.5:10:1, and other processes were normal.
[0109] In the examples and comparative examples, the polyether epoxy co-modified silicone oil emulsion was a mixture of polyether epoxy co-modified silicone oil, emulsifier, and deionized water in a mass ratio of 5:1:10; the emulsifier was a mixture of emulsifier OP-10 and APG1214 in a mass ratio of 2:1; and the thickness of both the inner layer and the outer layer in the examples and comparative examples was 1 mm.
[0110] Sources of raw materials used (for illustrative purposes only):
[0111] 40D / 24F-FDY Nylon Fiber (Moisture-wicking Fiber): Yiwu Huading Nylon Co., Ltd.; Emulsifier OP-10 (Industrial Grade): Etia; APG1214 (99%): Kandis Chemical (Hubei) Co., Ltd.; Antioxidant 3114: Hangzhou Jingyou Chemical Co., Ltd.; Semi-dull PET Chips BR8040: SK Korea; Dye S19049: Shanghai Yuanye Biotechnology Co., Ltd.; Polyether Epoxy Co-modified Silicone Oil Emulsion ETE301: Shandong Dayi Chemical Co., Ltd.; Carboxylated Carbon Nanotubes C493314, Polyvinylpyrrolidone P434439, Pyridine P111511, Hyperbranched Polyamide HyperN 103: Wuhan Hyperbranched Resin Technology Co., Ltd.; Triethanolamine T108151, Tetramethylammonium hydroxide pentahydrate T105041, γ-(2,3-epoxypropoxy)propyltrimethoxysilane G134407, DOPO (9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) D102416, Triphenylphosphine T104475, Gelatin G108394, Carboxymethyl chitosan C304738, Ethylene glycol E103319: Aladdin Reagent; Zinc acetate dihydrate, methanol, potassium hydroxide, thionyl chloride, N,N-dimethylformamide, toluene, sodium periodate, acetic acid, isopropanol, tert-butanol, analytical grade: commercially available.
[0112] Performance testing: The fabrics prepared in the examples and comparative examples were tested.
[0113] Flame retardancy: Limiting oxygen index was determined according to GB / T 5454-1997; Antibacterial properties: Staphylococcus aureus was used as the test strain, and the test was conducted according to GB / T20944.3-2008. The sample was washed with standard water 30 times, and then the antibacterial rate was tested; UV resistance: 4cm×4cm samples were cut, and UPF was tested according to GB / T 18830-2009; Air permeability: Air permeability was tested according to GB / T 5453, with a pressure difference of 100Pa; Color fastness to dry rubbing: The test was conducted according to GB / T 3920-2008, and the grade indicated the effect, with grade 5 being the best; Moisture absorption and quick-drying properties: The test was conducted according to GB / T 21655.1-2023, with grade III being the best. The results are shown in Table 1.
[0114] Table 1
[0115]
[0116] The invention provides a highly sun-protective, breathable, moisture-wicking, and quick-drying wrinkle fabric and its preparation method. Through process and component design, a green, environmentally friendly, flame-retardant, antibacterial, and antistatic highly sun-protective, breathable, moisture-wicking, and quick-drying wrinkle fabric is prepared. In Table 1, / indicates that it was not tested.
[0117] Comparing Example 3 with Comparative Example 1, it can be seen that in order to improve the mechanical strength and antistatic properties of matte or semi-matte polyester fibers, carboxylated carbon nanotubes are blended with matte or semi-matte PET chips and melt-spun to prepare matte or semi-matte polyester fibers. In order to improve the UV resistance and antibacterial properties of polyester fibers, carboxylated carbon nanotubes are used as the matrix and a solution method is used to prepare nano-zinc oxide composite carboxylated carbon nanotubes as composite nanoparticles. In order to improve the uniformity of the composite nanoparticles in polyester fibers, the composite nanoparticles are first subjected to acylation and then grafted with hyperbranched polyamide to obtain polyamine-modified composite carboxylated carbon nanotubes. In order to further improve the flame retardancy of polyester fibers, polyamine-modified composite carboxylated carbon nanotubes are grafted with epoxy POSS containing DOPO to obtain modified carboxylated carbon nanotubes.
[0118] The epoxy-based POSS containing DOPO was first prepared using γ-(2,3-epoxypropoxy)propyltrimethoxysilane as a raw material to obtain polyepoxy-based POSS, and then DOPO was grafted onto it to obtain POSS containing both DOPO and epoxy groups. This POSS was then grafted onto polyamino-modified composite carboxylated carbon nanotubes using an epoxy-amino reaction. Through the triple synergy of phosphorus, nitrogen, and silicon, highly efficient halogen-free flame retardancy was achieved. At the same time, the multiple active sites on the carboxylated carbon nanotubes were modified to improve the compatibility with polyester fiber matrix and achieve a long-lasting flame retardant and antibacterial effect.
[0119] A double-sided knitted base fabric is woven from modified polyester fiber using a double-sided knitting machine. The inner layer of the double-sided knitted base fabric is woven from modified polyester fiber, and the outer layer is formed by interlacing modified polyester fiber or nylon fiber. To improve the dye uptake rate of the base fabric, the base fabric is subjected to a two-dip and two-nip treatment with a dialdehyde carboxymethyl chitosan solution, followed by pre-drying and baking, and then dyeing treatment, thereby achieving dyeing depth and improving dye fastness. Carboxymethyl chitosan is a water-soluble chitosan derivative, wherein the dialdehyde carboxymethyl chitosan is obtained by oxidizing carboxymethyl chitosan with sodium periodate.
[0120] Comparing Example 3 with Comparative Example 2, it can be seen that in order to further improve the antibacterial, flame retardant, UV resistance, and moisture absorption and breathability of the fabric, and to fix the dyed pre-treated base fabric, a finishing agent was prepared using gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, modified carboxylated carbon nanotubes, and deionized water. This agent was used to treat the pre-treated base fabric. By controlling the mass ratio of gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, and modified carboxylated carbon nanotubes, a complex cross-linked network was constructed. At the same time, the modified carbon nanotubes were constructed through multi-level pores, which is beneficial to improving breathability and quick-drying properties. The introduction of polyether epoxy co-modified silicone oil emulsion maintained the soft touch of the fabric, thereby effectively balancing the needs of protection (flame retardancy, antibacterial, UV resistance, antistatic properties, etc.) and comfort.
[0121] The above description is merely an embodiment of the present invention and does not limit the patent scope of the present invention. Any equivalent structural transformations made using the present invention's specification under the inventive concept of the present invention, or direct / indirect applications in other related technical fields, are included within the patent protection scope of the present invention.
Claims
1. A method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric, characterized in that, Includes the following steps: S1: Modified carboxylated carbon nanotubes, antioxidants, and PET chips are dried, blended, melt-spun, cooled, and wound to obtain modified polyester fibers; S2: A double-sided knitted base fabric is woven from modified polyester fiber using a double-sided knitting machine; the inner layer of the double-sided knitted base fabric is woven from modified polyester fiber; the outer layer of the double-sided knitted base fabric is formed by interlacing modified polyester fiber or nylon fiber. S3: First, the double-sided knitted base fabric is subjected to two dips and two nips with a dialdehyde carboxymethyl chitosan solution, pre-drying and baking, then dyed with dye, soaped, washed with water and dried to obtain the pre-treated base fabric. S4: A finishing solution was prepared using gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, modified carboxylated carbon nanotubes, and deionized water. In the finishing solution, the mass ratio of gelatin, polyether epoxy co-modified silicone oil emulsion, dialdehyde carboxymethyl chitosan, and modified carboxylated carbon nanotubes is 3:0.5:12:
1. S5: The pre-treated base fabric is immersed in the finishing solution, then subjected to padding, wrinkling, shaping, and drying to obtain a strong sun protection, high breathability, moisture absorption and quick-drying wrinkled fabric. The preparation of modified carboxylated carbon nanotubes includes the following steps: (1) Mix zinc acetate dihydrate and methanol, add carboxylated carbon nanotubes and polyvinylpyrrolidone, sonicate for 8-10 min, heat to 58-60℃, add potassium hydroxide and methanol mixture, stir for 1-2 h, transfer to reaction vessel, keep at 178-180℃ for 11-12 h, filter, wash and dry to obtain composite carboxylated carbon nanotubes; (2) Under a nitrogen atmosphere, the composite carboxylated carbon nanotubes, thionyl chloride, and N,N-dimethylformamide were mixed and stirred at 68-72℃ for 22-24h. The mixture was then dried under reduced pressure and transferred to N,N-dimethylformamide. The mixture was then heated to 58-62℃ and ultrasonically dispersed for 25-30min. A mixed solution of pyridine, N,N-dimethylformamide, and hyperbranched polyamide was added and stirred at 18-25℃ for 22-24h. The mixture was then filtered, washed until neutral, dried, and ground to obtain the multi-amino modified composite carboxylated carbon nanotubes. (3) Mix polyamino-modified composite carboxylated carbon nanotubes, epoxy POSS containing DOPO, triethanolamine, and N,N-dimethylformamide, ultrasonically stir for 10-20 min, keep warm at 60-70℃ for 3-5 h, wash, and dry to obtain modified carboxylated carbon nanotubes.
2. The method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric according to claim 1, characterized in that, PET slices are either semi-dull or fully dull PET slices.
3. The method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying wrinkle-resistant fabric according to claim 1, characterized in that, In the preparation of modified polyester fibers, the mass ratio of antioxidant, modified carboxylated carbon nanotubes, and PET chips is 0.1:1:
99.
4. The method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric according to claim 1, characterized in that, The weight of double-knitted base fabric is 108-112 g / m². 2 .
5. The method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric according to claim 1, characterized in that, In step S4, the working conditions for the two-dip and two-nip treatment are: immersion time 60s, roll-off rate 100%; the pre-drying working conditions are: holding at 78-82℃ for 4-6min; the baking working conditions are: holding at 120-130℃ for 2-4min; the dyeing working conditions are: holding at 85-90℃ for 50-60min, liquor ratio 1:(40-55), pH 5.5; in step S6, the working conditions for the padding treatment are: three-dip and three-nip treatment, immersion time 90-100s, roll-off rate 80%; the wrinkling treatment working conditions are: temperature 180-200℃, pressure 5-15kg / cm. 2 The time is 10-30 seconds, and the wrinkling direction is either longitudinal or transverse.
6. The method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying wrinkle-resistant fabric according to claim 1, characterized in that, In the finishing solution, the ratio of dialdehyde carboxymethyl chitosan to deionized water is 1 g: (40-50) mL.
7. The method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric according to claim 1, characterized in that, The preparation of dialdehyde carboxymethyl chitosan includes the following steps: Carboxymethyl chitosan and deionized water were mixed, sodium periodate was added, the pH was adjusted to 3.5, and the mixture was stirred at 38-42℃ in the dark for 3-4 hours. Ethylene glycol was added, and the mixture was stirred at 18-25℃ for 20-30 minutes. The mixture was washed 3-5 times by centrifugation with tert-butanol, freeze-dried, and ground to obtain dialdehyde carboxymethyl chitosan.
8. The method for preparing a highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric according to claim 1, characterized in that, The preparation of DOPO-containing epoxy-based POSS includes the following steps: 1) Mix tetramethylammonium hydroxide pentahydrate, isopropanol, and deionized water, add a mixture of γ-(2,3-epoxypropoxy)propyltrimethoxysilane and isopropanol, stir at 28-32℃ for 6 hours, rotary evaporate, add toluene, heat to 88-90℃ and keep warm for 3-4 hours to obtain polyepoxy group POSS; 2) Mix polyepoxy group POSS, DOPO, triphenylphosphine and toluene, heat to 118-120℃ and hold for 110-130 min, then distill under reduced pressure and dry to obtain epoxy group POSS containing DOPO.
9. A highly sun-protective, breathable, moisture-wicking, quick-drying, wrinkle-resistant fabric, characterized in that... It is prepared by any one of the preparation methods in claims 1-8.