Warp-direction elastic tatting antibacterial fabric and preparation method thereof
By introducing composite polyester particles and modified antibacterial agents into warp-stretch woven fabrics, and combining electrospinning and blended spinning processes, the problems of poor antibacterial and mechanical properties of traditional woven fabrics have been solved, achieving efficient and long-lasting antibacterial effects and excellent mechanical properties.
Patent Information
- Application Number
- CN202511909273.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-17
- Publication Date
- 2026-03-20
AI Technical Summary
Traditional woven fabrics have poor antibacterial and mechanical properties. In particular, in warp elastic designs, antibacterial components are prone to falling off and are difficult to penetrate evenly. Furthermore, the hygroscopic nature of cellulose fibers promotes bacterial growth in humid environments. Existing technologies cannot achieve both elasticity and antibacterial properties.
A method for preparing composite polyester particles and modified antibacterial agents is adopted. The modified antibacterial agents are uniformly dispersed in composite polyester staple fibers through electrospinning process. Combined with the mixed spinning process of wool and spandex yarn, a warp-stretch woven fabric with high antibacterial and mechanical properties is formed.
It improves the environmental performance, mechanical properties and antibacterial properties of the fabric, enhances the durability and broad-spectrum antibacterial activity of the modified antibacterial agent, reduces the rate at which the modified antibacterial agent is lost due to friction and washing, and enhances the moisture absorption of the fabric.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of antibacterial fabric preparation technology, specifically relating to a warp-stretch woven antibacterial fabric and its preparation method. Background Technology
[0002] Traditional woven fabrics form a stable structure through warp and weft interlacing, while warp-elastic designs, through the introduction of elastic fibers such as spandex or special weaving processes, endow fabrics with longitudinal tensile recovery capabilities, making them widely used in sportswear, medical protective equipment, and other fields. However, improving their antibacterial properties has always faced technical bottlenecks, with the core issue stemming from the incompatibility between material properties and antibacterial processes. First, the surface chemical properties of elastic fibers differ significantly from those of conventional cotton and polyester substrates, making it difficult for traditional finishing processes such as silver ions and organic antibacterial agents to form stable adhesion on their surface, leading to the easy shedding of antibacterial components during washing or stretching. Second, while the tightness of the woven structure can improve physical protection, the dynamic changes in fiber gaps caused by warp elasticity make it difficult for antibacterial agents to penetrate evenly and form a long-lasting protective layer. In addition, high-temperature setting and other processing steps can easily cause the aggregation and failure of nano-sized antibacterial particles, and the repeated stretching and deformation of elastic fabrics during use further accelerates the decline of antibacterial function.
[0003] Patent CN111364146B discloses a warp-stretch woven fabric and its preparation method. This warp-stretch woven fabric comprises warp yarns and weft yarns. The warp yarns include pure spun cellulose yarns and / or blended yarns primarily composed of cellulose fibers, wherein the cellulose fiber content in the blended warp yarns is ≥50% and does not contain elastic yarns. The weft yarns include one or more combinations of pure cellulose fiber yarns, blended yarns primarily composed of cellulose fibers, and elastic yarns; wherein the cellulose fiber content in the blended weft yarns is ≥50%. The warp-stretch woven fabric prepared by this method has a warp elastic elongation of 10-15%, a residual elongation of 4-8%, and an elastic recovery rate of 55-85%, exhibiting similar comfortable elasticity to knitted fabrics. While this warp-stretch woven fabric possesses elasticity advantages, it has significant shortcomings in antibacterial properties. The warp and weft yarns are mainly made of cellulose fibers. While these natural fibers have some hygroscopic properties, their antibacterial mechanism relies primarily on physical adsorption and basic antibacterial effects. Their inhibition rate against common pathogens such as Staphylococcus aureus and Escherichia coli is typically less than 70%, and they are easily affected by environmental humidity. Especially in humid environments, the hygroscopic properties of cellulose fibers can actually provide a breeding ground for bacteria. Furthermore, if the weft yarns contain conventional spandex, its smooth chemical structure lacks antibacterial activity. Without the use of nano-silver composites or quaternary ammonium salt modification to impart lasting antibacterial function, the fabric's hygienic properties are further weakened. Summary of the Invention
[0004] The purpose of this invention is to provide a warp-stretch woven antibacterial fabric and its preparation method, which solves the technical problem of poor antibacterial and mechanical properties of fabrics in the prior art.
[0005] To achieve the above objectives, the present invention adopts the following technical solution: This invention provides a method for preparing a warp-stretch woven antibacterial fabric, comprising the following steps: Step 1: Add composite polyester particles to a mixed solution of N,N-dimethylformamide and acetone, heat and stir, add modified antibacterial agent, disperse ultrasonically, and then perform electrospinning to obtain a composite polyester fiber film. Dry, hot press, and cut to obtain composite polyester staple fiber. Step 2: Disinfect, wash and carbonize the wool to obtain pretreated wool. Mix the pretreated wool with composite polyester staple fiber evenly, add antistatic agent and emulsifying oil, open and mix, comb, draw and roving process to obtain composite woolen yarn. Step 3: Use spandex yarn as the core yarn, wrap it with pretreated wool to form an elastic covered yarn, mix the elastic covered yarn with the mixed coarse yarn, spin it, weave it, and heat set it to obtain a warp-stretch woven antibacterial fabric.
[0006] Preferably, the method for preparing the composite polyester particles in step one includes the following steps: Q1: Under nitrogen atmosphere, 2,5-furandicarboxylic acid is added to a container, followed by ethylene glycol and tetraisopropoxytitanium. The mixture is heated under a nitrogen atmosphere at normal pressure to obtain mixture 1. Q2: Under nitrogen atmosphere, 2,5-furandicarboxylic acid is added to a container, followed by diethylene glycol and tetraisopropoxytitanium. The mixture is heated under a nitrogen atmosphere at normal pressure to obtain mixture 2. Q3: Under nitrogen atmosphere, 2,5-furandicarboxylic acid was added to a container, followed by triethylene glycol and tetraisopropoxytitanium. The mixture was heated under a nitrogen atmosphere at normal pressure to obtain mixture 3. Q4: Under nitrogen atmosphere, mixture 1, mixture 2 and mixture 3 are added to the container in sequence, then tetraisopropoxy titanium and methanesulfonic acid are added. After heating and stirring under normal pressure nitrogen atmosphere, the reaction is carried out under reduced pressure. After the reaction is completed, the mixture is granulated and dried to obtain composite polyester particles.
[0007] The synthesis reaction formula for the composite polyester particles in the above process is as follows: Preferably, in Q1, the ratio of 2,5-furandicarboxylic acid, ethylene glycol, and tetraisopropoxytitanium is (18.82-21.62) g : (7.8-8.8) g : (0.112-0.12) g, and the heating reaction temperature is 200-220℃; in Q2, the ratio of 2,5-furandicarboxylic acid, diethylene glycol, and tetraisopropoxytitanium is (12.71-13.81) g : (9.11-9.69) g : (0.093-0.101) g, and the heating reaction temperature is 170-190℃.
[0008] Preferably, in Q3, the ratio of 2,5-furandicarboxylic acid, triethylene glycol, and tetraisopropoxytitanium is (12.71-13.81) g: (12.11-14.69) g: (0.113-0.119) g, and the heating reaction temperature is 170-190℃; in Q4, the ratio of mixture 1, mixture 2, mixture 3, tetraisopropoxytitanium, and methanesulfonic acid is (1.82-2.46) g: (1.62-2.02) g: (1.48-3.06) g: (0.016-0.021) g: (0.035-0.052) g, the heating and stirring reaction temperature is 180-190℃, the temperature for raising the temperature and reducing the pressure is 210-230℃, and the pressure is reduced to 20-22 Pa.
[0009] Preferably, the preparation method of the modified antibacterial agent includes the following steps: S1: 2-Iodoaniline, phenylacetylene, cuprous iodide, Pd(PPh3)Cl2 and triethylamine were added sequentially to a container. The reaction was carried out under a nitrogen atmosphere with stirring. After the reaction was completed, ethyl acetate was added for dilution, washing, drying, filtering, and purification under reduced pressure to obtain intermediate a. S2: Methyl anthranilate, intermediate a, triethoxymethane and ammonium chloride were added to a container, heated and stirred in an oil bath, cooled, distilled water was added, extracted, dried, filtered and purified to obtain intermediate b; S3: Intermediate b and N-fluorobisbenzenesulfonamide were added to acetonitrile, followed by the addition of cuprous iodide. The mixture was heated in an oil bath and reacted. After the reaction was completed, the mixture was cooled, extracted, dried, filtered, and purified to obtain the modified antibacterial agent.
[0010] In the above process, 2-iodoaniline and phenylacetylene were first used as raw materials to prepare intermediate a via a Sonogashira coupling reaction under the dual catalysis of cuprous iodide and Pd(PPh3)Cl2. Subsequently, methyl anthranilate and intermediate a were reacted in the presence of triethoxymethane and ammonium chloride to prepare intermediate b via cyclization condensation. Finally, intermediate b was fluorinated using N-fluorobisbenzenesulfonamide as an electrophilic fluorine source under the condition of cuprous iodide as a catalyst to prepare the modified antibacterial agent.
[0011] Preferably, in S1, the ratio of 2-iodoaniline, phenylacetylene, cuprous iodide, Pd(PPh3)Cl2 and triethylamine is (0.98-1.12) g : (0.58-0.62) mL : (0.13-0.19) g : (0.051-0.057) g : (18-22) mL, the stirring reaction temperature is 20-22℃, and the stirring reaction time is 3-5 h.
[0012] Preferably, in S2, the ratio of methyl anthranilate, intermediate a, triethoxymethane and ammonium chloride is (0.32-0.46) mL : (0.61-0.73) g : (0.522-0.648) mL : (0.12-0.24) g, the oil bath heating and stirring temperature is 95-100℃, and the stirring time is 2-3 h.
[0013] Preferably, in S3, the ratio of intermediate b, N-fluorobis(benzenesulfonamide), acetonitrile, and cuprous iodide is (0.028-0.036) g : (0.059-0.067) g : (1-1.5) mL : (0.0036-0.004) g, the oil bath heating reaction temperature is 90-110℃, and the reaction time is 6-8 h.
[0014] Preferably, in step one, the ratio of composite polyester particles, N,N-dimethylformamide, acetone, and modified antibacterial agent is (10-20) g : (70-90) mL : (20-30) mL : (0.1-0.3) g; the ultrasonic dispersion time is 30-45 min; during the electrospinning process, a high voltage of 12 kV is applied between the injector and the collector; the syringe injection speed is 1 mL / h; the winding speed of the collecting roller is 120 rpm; the electrospinning distance is 20 cm; and the hot-pressing temperature is 1... The temperature is 10-120℃, and the time is 30-35s. In step two, the ratio of pretreated wool, composite polyester staple fiber, antistatic agent and emulsified oil is (50-60)g:(40-50)g:(10-14)g:(10-18)g. In step three, the ratio of elastic covered yarn and mixed coarse yarn is (70-75)g:(24-32)g. During the spinning process, the warp twist is 80-100 twists / m and the weft twist is 50-70 twists / m. During the weaving process, a twill weave is used.
[0015] As a preferred embodiment, a warp-stretch woven antibacterial fabric is prepared using the above-described preparation method.
[0016] In summary, due to the adoption of the above technical solution, the beneficial effects of the present invention are: 1. This invention first uses 2,5-furandicarboxylic acid, ethylene glycol, diethylene glycol, and triethylene glycol as raw materials to prepare composite polyester particles. Subsequently, a modified antibacterial agent is prepared using 2-iodoaniline, phenylacetylene, methyl anthranilate, and N-fluorobisbenzenesulfonamide as raw materials. Adding the prepared composite polyester particles and the modified antibacterial agent to the preparation process of antibacterial fabric can effectively improve its environmental performance, mechanical properties, and antibacterial properties. The addition of wool can effectively reduce wrinkling and improve its moisture absorption properties.
[0017] 2. This invention applies the prepared composite polyester particles to the preparation process of warp-stretch woven antibacterial fabric, which can effectively improve the environmental performance and mechanical properties of the fabric. The 2,5-furandicarboxylic acid used in the composite polyester particles is derived from biomass conversion, replacing traditional petroleum-based materials and reducing dependence on fossil resources. Moreover, the furan ring structure is more easily degraded by microorganisms than the benzene ring, thereby reducing the environmental retention of polyester. At the same time, the polyester prepared by different chain lengths forms a complex chain structure. Short chains provide high crystallinity, strength, and modulus, while long chains improve flexibility and elongation at break, achieving complementary properties, thus endowing the fabric with both environmental sustainability and excellent mechanical properties.
[0018] 3. The present invention adds the prepared modified antibacterial agent to the preparation process of warp-stretch woven antibacterial fabric, which can effectively improve its antibacterial performance. The modified antibacterial agent has efficient and long-lasting broad-spectrum antibacterial properties. At the same time, by uniformly dispersing and embedding the modified antibacterial agent in the composite polyester staple fiber through electrospinning process, the rate at which the modified antibacterial agent is lost due to friction and washing can be reduced, thereby improving its antibacterial durability. Detailed Implementation
[0019] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0020] Example 1: This example discloses a method for preparing composite polyester particles, including the following steps: Q1: Under nitrogen atmosphere, 20.52g of 2,5-furandicarboxylic acid was added to a container, followed by 8.3g of ethylene glycol and 0.116g of tetraisopropoxytitanium. The mixture was heated at 220℃ under normal nitrogen atmosphere to obtain mixture 1. Q2: Under nitrogen atmosphere, 13.31g of 2,5-furandicarboxylic acid was added to a container, followed by 9.4g of diethylene glycol and 0.097g of tetraisopropoxytitanium. The mixture was heated at 180°C under normal nitrogen atmosphere to obtain mixture 2. Q3: Under nitrogen atmosphere, 13.11g of 2,5-furandicarboxylic acid was added to a container, followed by 13.4g of triethylene glycol and 0.116g of tetraisopropoxytitanium. The mixture was heated at 180°C under normal nitrogen atmosphere to obtain mixture 3. Q4: Under nitrogen atmosphere, 2.14g of mixture 1, 1.82g of mixture 2 and 2.26g of mixture 3 were added to a container in sequence. Then, 0.018g of tetraisopropoxytitanium and 0.043g of methanesulfonic acid were added. The mixture was heated and stirred at 180°C under normal pressure and nitrogen atmosphere. The temperature was then raised to 220°C and the pressure was reduced to 20Pa. After the reaction was completed, the mixture was granulated and dried to obtain composite polyester particles.
[0021] This embodiment discloses a method for preparing a modified antibacterial agent, including the following steps: S1: 1.05g of 2-iodoaniline, 0.6g of phenylacetylene, 0.15g of cuprous iodide, 0.054g of Pd(PPh3)Cl2 and 20mL of triethylamine were added sequentially to a container. The mixture was stirred at 20°C for 4 hours under a nitrogen atmosphere. After the reaction was completed, ethyl acetate was added for dilution, followed by washing, drying, filtration, and purification under reduced pressure to obtain intermediate a. S2: Add 0.39 mL of methyl anthranilate, 0.66 g of intermediate a, 0.585 mL of triethoxymethane and 0.18 g of ammonium chloride to a container, heat and stir in an oil bath at 100 °C for 3 h, cool, add distilled water, extract, dry, filter, and purify to obtain intermediate b; S3: 0.032 g intermediate b and 0.063 g N-fluorobisbenzenesulfonamide were added to 1.25 mL acetonitrile, followed by 0.0038 g cuprous iodide. The mixture was heated in an oil bath at 100 °C for 6 h. After the reaction was completed, the mixture was cooled, extracted, dried, filtered, and purified to obtain the modified antibacterial agent.
[0022] This embodiment discloses a method for preparing a warp-stretch woven antibacterial fabric, including the following steps: Step 1: Add 15g of composite polyester particles to a mixed solution of 80mL N,N-dimethylformamide and 25mL acetone. After heating and stirring, add 0.2g of modified antibacterial agent. After ultrasonic dispersion for 30min, perform electrospinning treatment. During the electrospinning treatment, use HZ-12 type electrospinning equipment (Huizhi Electrospinning). Apply a high voltage of 12kV between the injector and the collector. The syringe injection speed is 1mL / h, the winding speed of the collecting roller is 120rpm, and the electrospinning distance is 20cm to obtain a composite polyester fiber film. Dry the film, hot press it at 120℃ for 35s, and cut it to obtain composite polyester staple fibers. Step 2: Disinfect, wash and carbonize the wool to obtain pretreated wool. Mix 55g of pretreated wool with 45g of composite polyester staple fiber evenly, add 12g of cocamidopropyl betaine and 14g of castor oil, open and mix, comb, draw, and roving to obtain mixed coarse yarn. Step 3: Use spandex yarn as the core yarn, wrap it with pretreated wool to form an elastic covered yarn. Mix 72.5g of elastic covered yarn with 28g of mixed coarse yarn and spin it. During the spinning process, the warp twist is 90 twists / m and the weft twist is 60 twists / m. Then, weave it with a twill weave and heat set it to obtain a warp elastic woven antibacterial fabric.
[0023] Example 2: This example discloses a method for preparing composite polyester particles, including the following steps: Q1: Under nitrogen atmosphere, 18.82g of 2,5-furandicarboxylic acid was added to a container, followed by 8.8g of ethylene glycol and 0.112g of tetraisopropoxytitanium. The mixture was heated at 220℃ under normal pressure and nitrogen atmosphere to obtain mixture 1. Q2: Under nitrogen atmosphere, 12.71g of 2,5-furandicarboxylic acid was added to a container, followed by 9.11g of diethylene glycol and 0.093g of tetraisopropoxytitanium. The mixture was heated at 180°C under normal nitrogen atmosphere to obtain mixture 2. Q3: Under nitrogen atmosphere, 12.71g of 2,5-furandicarboxylic acid was added to a container, followed by 12.11g of triethylene glycol and 0.113g of tetraisopropoxytitanium. The mixture was heated at 180°C under normal nitrogen atmosphere to obtain mixture 3. Q4: Under nitrogen atmosphere, 2.46g of mixture 1, 1.62g of mixture 2 and 1.48g of mixture 3 were added to a container in sequence, followed by 0.016g of tetraisopropoxytitanium and 0.035g of methanesulfonic acid. The mixture was heated and stirred at 180°C under normal nitrogen atmosphere, then heated to 220°C and depressurized to 20Pa to react. After the reaction was completed, the mixture was granulated and dried to obtain composite polyester particles.
[0024] This embodiment discloses a method for preparing a modified antibacterial agent, including the following steps: S1: 0.98 g 2-iodoaniline, 0.58 g phenylacetylene, 0.19 g cuprous iodide, 0.057 g Pd(PPh3)Cl2 and 22 mL triethylamine were added sequentially to a container. The mixture was stirred at 20 °C for 4 h under a nitrogen atmosphere. After the reaction was completed, ethyl acetate was added for dilution, followed by washing, drying, filtration, and purification under reduced pressure to obtain intermediate a. S2: Add 0.32 mL of methyl anthranilate, 0.61 g of intermediate a, 0.522 mL of triethoxymethane and 0.12 g of ammonium chloride to a container, heat and stir in an oil bath at 100 °C for 3 h, cool, add distilled water, extract, dry, filter, and purify to obtain intermediate b; S3: Add 0.028g of intermediate b and 0.059g of N-fluorobisbenzenesulfonamide to 1mL of acetonitrile, then add 0.0036g of cuprous iodide, heat in an oil bath at 100℃ for 6h, cool, extract, dry, filter, and purify to obtain the modified antibacterial agent.
[0025] This embodiment discloses a method for preparing a warp-stretch woven antibacterial fabric, including the following steps: Step 1: Add 10g of composite polyester particles to a mixed solution of 90mL N,N-dimethylformamide and 20mL acetone. After heating and stirring, add 0.1g of modified antibacterial agent. After ultrasonic dispersion for 30min, perform electrospinning treatment. During the electrospinning treatment, use HZ-12 type electrospinning equipment (Huizhi Electrospinning). Apply a high voltage of 12kV between the injector and the collector. The syringe injection speed is 1mL / h, the winding speed of the collecting roller is 120rpm, and the electrospinning distance is 20cm to obtain a composite polyester fiber film. Dry, hot press at 120℃ for 35s, and cut to obtain composite polyester short fibers. Step 2: Disinfect, wash and carbonize the wool to obtain pretreated wool. Mix 60g of pretreated wool with 40g of composite polyester staple fiber evenly, add 10g of cocamidopropyl betaine and 18g of castor oil, open and mix, comb, draw, and roving to obtain mixed coarse yarn. Step 3: Use spandex yarn as the core yarn, wrap it with pretreated wool to form an elastic covered yarn. Mix 70g of elastic covered yarn with 24g of mixed coarse yarn and spin it. During the spinning process, the warp twist is 90 twists / m and the weft twist is 60 twists / m. Then, weave it with a twill weave and heat set it to obtain a warp elastic woven antibacterial fabric.
[0026] Example 3: This example discloses a method for preparing composite polyester particles, including the following steps: Q1: Under nitrogen atmosphere, 21.62g of 2,5-furandicarboxylic acid was added to a container, followed by 7.8g of ethylene glycol and 0.12g of tetraisopropoxytitanium. The mixture was heated at 220℃ under normal pressure and nitrogen atmosphere to obtain mixture 1. Q2: Under nitrogen atmosphere, 13.81g of 2,5-furandicarboxylic acid was added to a container, followed by 9.69g of diethylene glycol and 0.101g of tetraisopropoxytitanium. The mixture was heated at 180°C under normal nitrogen atmosphere to obtain mixture 2. Q3: Under nitrogen atmosphere, 13.81g of 2,5-furandicarboxylic acid was added to a container, followed by 14.69g of triethylene glycol and 0.119g of tetraisopropoxytitanium. The mixture was heated at 180°C under normal nitrogen atmosphere to obtain mixture 3. Q4: Under nitrogen atmosphere, 1.82g of mixture 1, 2.02g of mixture 2 and 3.06g of mixture 3 were added to a container in sequence. Then, 0.021g of tetraisopropoxytitanium and 0.052g of methanesulfonic acid were added. The mixture was heated and stirred at 180°C under normal pressure nitrogen atmosphere. The temperature was then raised to 220°C and the pressure was reduced to 20Pa to react. After the reaction was completed, the mixture was granulated and dried to obtain composite polyester particles.
[0027] This embodiment discloses a method for preparing a modified antibacterial agent, including the following steps: S1: 1.12 g 2-iodoaniline, 0.62 g phenylacetylene, 0.13 g cuprous iodide, 0.051 g Pd(PPh3)Cl2 and 18 mL triethylamine were added sequentially to a container. The mixture was stirred at 20 °C for 4 h under a nitrogen atmosphere. After the reaction was completed, ethyl acetate was added for dilution, followed by washing, drying, filtration, and purification under reduced pressure to obtain intermediate a. S2: Add 0.46 mL of methyl anthranilate, 0.73 g of intermediate a, 0.648 mL of triethoxymethane and 0.24 g of ammonium chloride to a container, heat and stir in an oil bath at 100 °C for 3 h, cool, add distilled water, extract, dry, filter, and purify to obtain intermediate b; S3: 0.036 g of intermediate b and 0.067 g of N-fluorobisbenzenesulfonamide were added to 1.5 mL of acetonitrile, followed by 0.004 g of cuprous iodide. The mixture was heated in an oil bath at 100 °C for 6 h. After the reaction was completed, the mixture was cooled, extracted, dried, filtered, and purified to obtain the modified antibacterial agent.
[0028] This embodiment discloses a method for preparing a warp-stretch woven antibacterial fabric, including the following steps: Step 1: Add 20g of composite polyester particles to a mixed solution of 70mL N,N-dimethylformamide and 30mL acetone. After heating and stirring, add 0.3g of modified antibacterial agent. After ultrasonic dispersion for 30min, perform electrospinning treatment. During the electrospinning treatment, use HZ-12 type electrospinning equipment (Huizhi Electrospinning). Apply a high voltage of 12kV between the injector and the collector. The syringe injection speed is 1mL / h, the winding speed of the collecting roller is 120rpm, and the electrospinning distance is 20cm to obtain a composite polyester fiber film. Dry, hot press at 120℃ for 35s, and cut to obtain composite polyester staple fibers. Step 2: Disinfect, wash and carbonize the wool to obtain pretreated wool. Mix 50g of pretreated wool with 50g of composite polyester staple fiber evenly, add 14g of cocamidopropyl betaine and 18g of castor oil, open and mix, comb, draw, and roving to obtain mixed coarse yarn. Step 3: Use spandex yarn as the core yarn, wrap it with pretreated wool to form an elastic covered yarn. Mix 75g of elastic covered yarn with 32g of mixed coarse yarn and spin it. During the spinning process, the warp twist is 90 twists / m and the weft twist is 60 twists / m. Then, weave it with a twill weave and heat set it to obtain a warp elastic woven antibacterial fabric.
[0029] Example 4: This example discloses a method for preparing composite polyester particles, including the following steps: Q1: Under nitrogen atmosphere, 19.13g of 2,5-furandicarboxylic acid was added to a container, followed by 8.1g of ethylene glycol and 0.118g of tetraisopropoxytitanium. The mixture was heated at 220℃ under normal nitrogen atmosphere to obtain mixture 1. Q2: Under nitrogen atmosphere, 12.91g of 2,5-furandicarboxylic acid was added to a container, followed by 9.23g of diethylene glycol and 0.095g of tetraisopropoxytitanium. The mixture was heated at 180°C under normal nitrogen atmosphere to obtain mixture 2. Q3: Under nitrogen atmosphere, 12.94g of 2,5-furandicarboxylic acid was added to a container, followed by 12.87g of triethylene glycol and 0.114g of tetraisopropoxytitanium. The mixture was heated at 180°C under normal nitrogen atmosphere to obtain mixture 3. Q4: Under nitrogen atmosphere, 2.27g of mixture 1, 1.71g of mixture 2 and 1.87g of mixture 3 were added to a container in sequence, followed by 0.017g of tetraisopropoxytitanium and 0.038g of methanesulfonic acid. The mixture was heated and stirred at 180°C under normal pressure nitrogen atmosphere, then heated to 220°C and depressurized to 20Pa to react. After the reaction was completed, the mixture was granulated and dried to obtain composite polyester particles.
[0030] This embodiment discloses a method for preparing a modified antibacterial agent, including the following steps: S1: 1.03 g 2-iodoaniline, 0.59 g phenylacetylene, 0.14 g cuprous iodide, 0.053 g Pd(PPh3)Cl2 and 21 mL triethylamine were added sequentially to a container. The mixture was stirred at 20 °C for 4 h under a nitrogen atmosphere. After the reaction was completed, ethyl acetate was added for dilution, followed by washing, drying, filtration, and purification under reduced pressure to obtain intermediate a. S2: Add 0.35 mL of methyl anthranilate, 0.64 g of intermediate a, 0.551 mL of triethoxymethane and 0.15 g of ammonium chloride to a container, heat and stir in an oil bath at 100 °C for 3 h, cool, add distilled water, extract, dry, filter, and purify to obtain intermediate b; S3: Add 0.03g intermediate b and 0.061g N-fluorobisbenzenesulfonamide to 1.1mL acetonitrile, then add 0.0037g cuprous iodide, heat in an oil bath at 100℃ for 6h, cool, extract, dry, filter, and purify to obtain the modified antibacterial agent.
[0031] This embodiment discloses a method for preparing a warp-stretch woven antibacterial fabric, including the following steps: Step 1: Add 12g of composite polyester particles to a mixed solution of 75mL N,N-dimethylformamide and 22mL acetone. After heating and stirring, add 0.15g of modified antibacterial agent. After ultrasonic dispersion for 30min, perform electrospinning treatment. During the electrospinning treatment, use HZ-12 type electrospinning equipment (Huizhi Electrospinning). Apply a high voltage of 12kV between the injector and the collector. The injection speed of the syringe is 1mL / h, the winding speed of the collecting roller is 120rpm, and the electrospinning distance is 20cm to obtain a composite polyester fiber film. Dry the film, hot press it at 120℃ for 35s, and cut it to obtain composite polyester staple fibers. Step 2: Disinfect, wash and carbonize the wool to obtain pretreated wool. Mix 52g of pretreated wool with 48g of composite polyester staple fiber evenly, add 11g of cocamidopropyl betaine and 16g of castor oil, open and mix, comb, draw, and roving to obtain mixed coarse yarn. Step 3: Use spandex yarn as the core yarn, wrap it with pretreated wool to form an elastic covered yarn. Mix 71g of elastic covered yarn with 26g of mixed coarse yarn and spin it. During the spinning process, the warp twist is 90 twists / m and the weft twist is 60 twists / m. Then, weave it with a twill weave and heat set it to obtain a warp elastic woven antibacterial fabric.
[0032] Example 5: This example discloses a method for preparing composite polyester particles, including the following steps: Q1: Under nitrogen atmosphere, 20.87g of 2,5-furandicarboxylic acid was added to a container, followed by 8.5g of ethylene glycol and 0.114g of tetraisopropoxytitanium. The mixture was heated at 220℃ under normal pressure and nitrogen atmosphere to obtain mixture 1. Q2: Under nitrogen atmosphere, 13.78g of 2,5-furandicarboxylic acid was added to a container, followed by 9.51g of diethylene glycol and 0.099g of tetraisopropoxytitanium. The mixture was heated at 180°C under normal nitrogen atmosphere to obtain mixture 2. Q3: Under nitrogen atmosphere, 13.47g of 2,5-furandicarboxylic acid was added to a container, followed by 13.95g of triethylene glycol and 0.117g of tetraisopropoxytitanium. The mixture was heated at 180°C under normal nitrogen atmosphere to obtain mixture 3. Q4: Under nitrogen atmosphere, 2.01g of mixture 1, 1.93g of mixture 2 and 2.93g of mixture 3 were added to a container in sequence, followed by 0.02g of tetraisopropoxytitanium and 0.048g of methanesulfonic acid. The mixture was heated and stirred at 180°C under normal nitrogen atmosphere, then heated to 220°C and depressurized to 20Pa. After the reaction was completed, the mixture was granulated and dried to obtain composite polyester particles.
[0033] This embodiment discloses a method for preparing a modified antibacterial agent, including the following steps: S1: 1.09 g 2-iodoaniline, 0.61 g phenylacetylene, 0.18 g cuprous iodide, 0.056 g Pd(PPh3)Cl2 and 19 mL triethylamine were added sequentially to a container. The mixture was stirred at 20 °C for 4 h under a nitrogen atmosphere. After the reaction was completed, ethyl acetate was added for dilution, followed by washing, drying, filtration, and purification under reduced pressure to obtain intermediate a. S2: Add 0.43 mL of methyl anthranilate, 0.71 g of intermediate a, 0.631 mL of triethoxymethane and 0.21 g of ammonium chloride to a container, heat and stir in an oil bath at 100 °C for 3 h, cool, add distilled water, extract, dry, filter, and purify to obtain intermediate b; S3: 0.034 g of intermediate b and 0.065 g of N-fluorobisbenzenesulfonamide were added to 1.4 mL of acetonitrile, followed by 0.0039 g of cuprous iodide. The mixture was heated in an oil bath at 100 °C for 6 h. After the reaction was completed, the mixture was cooled, extracted, dried, filtered, and purified to obtain the modified antibacterial agent.
[0034] This embodiment discloses a method for preparing a warp-stretch woven antibacterial fabric, including the following steps: Step 1: Add 18g of composite polyester particles to a mixed solution of 85mL N,N-dimethylformamide and 28mL acetone. After heating and stirring, add 0.25g of modified antibacterial agent. After ultrasonic dispersion for 30min, perform electrospinning treatment. During the electrospinning treatment, use HZ-12 type electrospinning equipment (Huizhi Electrospinning). Apply a high voltage of 12kV between the injector and the collector. The injection speed of the syringe is 1mL / h, the winding speed of the collecting roller is 120rpm, and the electrospinning distance is 20cm to obtain a composite polyester fiber film. Dry the film, hot press it at 120℃ for 35s, and cut it to obtain composite polyester staple fibers. Step 2: Disinfect, wash and carbonize the wool to obtain pretreated wool. Mix 58g of pretreated wool with 42g of composite polyester staple fiber evenly, add 13g of cocamidopropyl betaine and 15g of castor oil, open and mix, comb, draw, and roving to obtain mixed coarse yarn. Step 3: Use spandex yarn as the core yarn, wrap it with pretreated wool to form an elastic covered yarn. Mix 74g of elastic covered yarn with 30g of mixed coarse yarn and spin it. During the spinning process, the warp twist is 90 twists / m and the weft twist is 60 twists / m. Then, weave it with a twill weave and heat set it to obtain a warp elastic woven antibacterial fabric.
[0035] Comparative Example 1: Compared with Example 1, Comparative Example 1 used cotton fibers instead of composite polyester particles in the process of preparing warp-stretch antibacterial fabric, while keeping other conditions unchanged.
[0036] Comparative Example 2: Compared with Example 1, Comparative Example 2 did not add any modified antibacterial agent during the preparation of warp elastic woven antibacterial fabric, and all other conditions remained unchanged.
[0037] The warp-stretch woven antibacterial fabrics prepared in Examples 1-5 and Comparative Examples 1-2 were subjected to performance tests. The tensile properties of the samples were tested according to GB / T 3923.1-2013, the tear properties according to GB / T 3917.1-2009, and the antibacterial properties according to GB / T 20944.1-2007. The test results are shown in Table 1. Table 1 According to GB / T 20944.1-2007, when the inhibition band width is greater than 1 mm and there is no bacterial growth under the sample, or when the inhibition band is within 1 mm and there is no bacterial growth, or when there is no inhibition band and no bacterial growth, it indicates that the sample has a good antibacterial effect; when the inhibition band width is 0 mm and there are only a few colonies with almost inhibited growth, it indicates that the sample has a good antibacterial effect; when the inhibition band width is 0 mm and there is moderate colony growth, with half the growth compared to the control sample, it indicates that the sample has a limited antibacterial effect; when the inhibition band width is 0 mm and there is a large number of colonies growing, with no or only slight reduction in growth compared to the control sample, it indicates that the sample has no antibacterial effect. As shown in Table 1, the test results indicate that the methods described in Examples 1-5 can effectively improve the mechanical and antibacterial properties of the fabric. A comparison between Comparative Example 1 and Examples 1-5 reveals that adding composite polyester particles can effectively improve the mechanical properties of the fabric. A comparison between Comparative Example 2 and Examples 1-5 shows that adding modified antibacterial agents can effectively improve the antibacterial properties of the fabric. The antibacterial band width in Comparative Example 1 is slightly lower than that in Examples 1-5. This is because cotton fibers are used instead of composite polyester particles. Cotton fibers have excellent hydrophilicity and easily absorb antibacterial agents, but their natural fiber structure lacks interaction with modified antibacterial agents. This may cause some modified antibacterial agents to migrate or detach during electrospinning or hot pressing, resulting in a lower concentration of antibacterial agents ultimately adhering to the fiber surface and a smaller antibacterial band width.
[0038] The above description is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any equivalent substitutions or modifications made by those skilled in the art within the scope of the technology disclosed in the present invention, based on the technical solution and inventive concept of the present invention, should be covered within the scope of protection of the present invention.
[0039] The preferred embodiments of the present invention disclosed above are merely illustrative of the invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the invention to specific implementations. Clearly, many modifications and variations can be made based on the content of this specification. This specification selects and specifically describes these embodiments to better explain the principles and practical applications of the invention, thereby enabling those skilled in the art to better understand and utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims
1. A method for preparing a warp-stretch woven antibacterial fabric, characterized in that, Includes the following steps: Step 1: Add composite polyester particles to a mixed solution of N,N-dimethylformamide and acetone, heat and stir, add modified antibacterial agent, disperse ultrasonically, and then perform electrospinning to obtain a composite polyester fiber film. Dry, hot press, and cut to obtain composite polyester staple fiber. Step 2: Disinfect, wash and carbonize the wool to obtain pretreated wool. Mix the pretreated wool with composite polyester staple fiber evenly, add antistatic agent and emulsifying oil, open and mix, comb, draw and roving process to obtain composite woolen yarn. Step 3: Use spandex yarn as the core yarn, wrap it with pretreated wool to form an elastic covered yarn, mix the elastic covered yarn with the mixed coarse yarn, spin it, weave it, and heat set it to obtain a warp-stretch woven antibacterial fabric.
2. The method for preparing a warp-stretch woven antibacterial fabric according to claim 1, characterized in that, In step one, the method for preparing the composite polyester particles, Includes the following steps: Q1: Under nitrogen atmosphere, 2,5-furandicarboxylic acid is added to a container, followed by ethylene glycol and tetraisopropoxytitanium. The mixture is heated under a nitrogen atmosphere at normal pressure to obtain mixture 1. Q2: Under nitrogen atmosphere, 2,5-furandicarboxylic acid is added to a container, followed by diethylene glycol and tetraisopropoxytitanium. The mixture is heated under a nitrogen atmosphere at normal pressure to obtain mixture 2. Q3: Under nitrogen atmosphere, 2,5-furandicarboxylic acid was added to a container, followed by triethylene glycol and tetraisopropoxytitanium. The mixture was heated under a nitrogen atmosphere at normal pressure to obtain mixture 3. Q4: Under nitrogen atmosphere, mixture 1, mixture 2 and mixture 3 are added to the container in sequence, then tetraisopropoxy titanium and methanesulfonic acid are added. After heating and stirring under normal pressure nitrogen atmosphere, the reaction is carried out under reduced pressure. After the reaction is completed, the mixture is granulated and dried to obtain composite polyester particles.
3. The method for preparing a warp-stretch woven antibacterial fabric according to claim 2, characterized in that, In Q1, the ratio of 2,5-furandicarboxylic acid, ethylene glycol, and tetraisopropoxytitanium is (18.82-21.62) g : (7.8-8.8) g : (0.112-0.12) g; in Q2, the ratio of 2,5-furandicarboxylic acid, diethylene glycol, and tetraisopropoxytitanium is (12.71-13.81) g : (9.11-9.69) g : (0.093-0.101) g.
4. The method for preparing a warp-stretch woven antibacterial fabric according to claim 2, characterized in that, In Q3, the ratio of 2,5-furandicarboxylic acid, triethylene glycol, and tetraisopropoxytitanium is (12.71-13.81) g : (12.11-14.69) g : (0.113-0.119) g; in Q4, the ratio of mixture 1, mixture 2, mixture 3, tetraisopropoxytitanium, and methanesulfonic acid is (1.82-2.46) g : (1.62-2.02) g : (1.48-3.06) g : (0.016-0.021) g : (0.035-0.052) g.
5. The method for preparing a warp-stretch woven antibacterial fabric according to claim 1, characterized in that, The preparation method of the modified antibacterial agent includes the following steps: S1: 2-Iodoaniline, phenylacetylene, cuprous iodide, Pd(PPh3)Cl2 and triethylamine were added sequentially to a container. The reaction was carried out under a nitrogen atmosphere with stirring. After the reaction was completed, ethyl acetate was added for dilution, washing, drying, filtering, and purification under reduced pressure to obtain intermediate a. S2: Methyl anthranilate, intermediate a, triethoxymethane and ammonium chloride were added to a container, heated and stirred in an oil bath, cooled, distilled water was added, extracted, dried, filtered and purified to obtain intermediate b; S3: Intermediate b and N-fluorobisbenzenesulfonamide were added to acetonitrile, followed by the addition of cuprous iodide. The mixture was heated in an oil bath and reacted. After the reaction was completed, the mixture was cooled, extracted, dried, filtered, and purified to obtain the modified antibacterial agent.
6. The method for preparing a warp-stretch woven antibacterial fabric according to claim 5, characterized in that, In S1, the ratio of the amounts of 2-iodoaniline, phenylacetylene, cuprous iodide, Pd(PPh3)Cl2 and triethylamine is (0.98-1.12) g : (0.58-0.62) mL : (0.13-0.19) g : (0.051-0.057) g : (18-22) mL.
7. The method for preparing a warp-stretch woven antibacterial fabric according to claim 5, characterized in that, In S2, the ratio of methyl anthranilate, intermediate a, triethoxymethane and ammonium chloride is (0.32-0.46) mL : (0.61-0.73) g : (0.522-0.648) mL : (0.12-0.24) g.
8. The method for preparing a warp-stretch woven antibacterial fabric according to claim 5, characterized in that, In S3, the ratio of intermediate b, N-fluorobis(benzenesulfonamide), acetonitrile and cuprous iodide is (0.028-0.036) g : (0.059-0.067) g : (1-1.5) mL : (0.0036-0.004) g.
9. The method for preparing a warp-stretch woven antibacterial fabric according to claim 1, characterized in that, In step one, the ratio of composite polyester particles, N,N-dimethylformamide, acetone and modified antibacterial agent is (10-20) g: (70-90) mL: (20-30) mL: (0.1-0.3) g. During the electrospinning process, a high voltage of 12kV is applied between the injector and the collector, the syringe injection speed is 1 mL / h, the winding speed of the collecting roller is 120 rpm, and the electrospinning distance is 20 cm. In step two, the ratio of pretreated wool, composite polyester staple fiber, antistatic agent and emulsified oil is (50-60) g: (40-50) g: (10-14) g: (10-18) g. In step three, the ratio of elastic covered yarn and mixed coarse yarn is (70-75) g: (24-32) g.
10. A warp-stretch woven antibacterial fabric, characterized in that, It is prepared by the preparation method according to any one of claims 1-9.
Citation Information
Patent Citations
A warp-stretch woven fabric and its preparation method
CN111364146B
