Lyocell fiber and polyester fiber blended yarn and preparation method and application thereof
Through modification treatment and nanoload technology, the wear resistance and antibacterial properties of Lycel fiber and polyester fiber blended yarns are improved, and the problems of wool and insufficient antibacterial properties of denim fabrics are solved, thus achieving higher quality yarns Performance and fabric functionality.
Patent Information
- Application Number
- CN202411661627.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-20
- Publication Date
- 2025-01-07
AI Technical Summary
The existing lycel fiber and polyester fiber blended yarns have poor wear resistance, resulting in the prepared denim fabrics that are easy to blew and pill, affecting aesthetics and service life, and lack of skin-friendly and antibacterial properties, which cannot meet high-quality denim Fabric demand.
By modifying the polyester fiber and lyceler fiber, nanotitanium dioxide loading and surface modification is carried out using chemical substances such as butyl titanate, silver nitrate and silane coupling agents, and combined with specific yarn modification liquid components to enhance the fiber Mechanical strength and antibacterial properties, and improve antistatic and wrinkle properties through silicone and quaternary ammonium groups in the yarn modification solution.
It significantly improves the wear resistance, antibacteriality and anti-flushing and pilling properties of the blended yarn, so that the prepared denim fabric has better wear comfort and functionality, and can meet the needs of high-quality denim fabrics.
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Figure BDA0005143539270000161
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of textiles, and in particular to a lyocell fiber and polyester fiber blended yarn and a preparation method and application thereof. Background Art
[0002] As one of the classic textiles, denim fabric is deeply loved by consumers for its unique texture and style. However, with the enhancement of environmental awareness and the diversification of consumer demand, traditional denim fabrics face challenges in performance, comfort and environmental protection. Lyocell fiber has excellent properties, such as high strength, good moisture absorption and breathability, but it also has some shortcomings, such as smooth fiber surface and poor fiber cohesion. Polyester fiber has the advantages of high strength, high modulus, good heat resistance, but poor moisture absorption. Therefore, blending lyocell fiber with polyester fiber can combine the advantages of both, make up for their respective shortcomings, and obtain blended yarn with excellent performance. Therefore, combining these two fibers through modification technology and applying them to denim fabrics has become an important way to solve the above problems.
[0003] However, there are some problems with the existing blended yarn preparation methods. For example, poor wear resistance causes the prepared denim fabric to be prone to pilling, affecting the aesthetics and service life. In addition, the skin-friendly and antibacterial properties need to be improved, resulting in the inability to meet people's demand for high-quality denim fabrics. Summary of the invention
[0004] In order to overcome the above-mentioned technical problems, the purpose of the present invention is to provide a lyocell fiber and polyester fiber blended yarn and a preparation method and application thereof, which solves the problem that the existing blended yarn has poor wear resistance, resulting in the prepared denim fabric being easy to pilling, affecting the aesthetics and service life, and the skin-friendly performance and antibacterial properties need to be improved, resulting in the inability to meet people's demand for high-quality denim fabrics.
[0005] The purpose of the present invention can be achieved through the following technical solutions:
[0006] A lyocell fiber and polyester fiber blended yarn comprises the following components in parts by weight:
[0007] 50-70 parts of modified polyester fiber, 30-50 parts of lyocell fiber;
[0008] Wherein, the modified polyester fiber is prepared by the following steps:
[0009] Step a1: adding polyester fiber and sodium hydroxide solution to a three-necked flask equipped with a stirrer and a thermometer, stirring the reaction for 20-30 minutes at a temperature of 25-30° C. and a stirring rate of 300-400 r / min, then heating to 65-75° C. and continuing stirring the reaction for 1-1.5 hours, cooling the reaction product to room temperature after the reaction, then vacuum filtering, washing the filter cake with distilled water for 2-3 times, then placing it in a vacuum drying oven, and drying it at a temperature of 50-55° C. for 2-3 hours to obtain alkali-treated polyester fiber;
[0010] Step a2: adding butyl titanate, silver nitrate and ethanol solution to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, stirring and reacting for 20-30 minutes at a temperature of 25-30° C. and a stirring rate of 300-400 r / min, then adding alkali-treated polyester fiber and heating to reflux and continuing stirring and reacting for 3-5 hours, after the reaction is completed, cooling the reaction product to room temperature, then vacuum filtering, washing the filter cake with anhydrous ethanol, anhydrous acetone and distilled water for 3-5 times in sequence, then placing it in a vacuum drying oven, and drying it at a temperature of 60-65° C. for 4-5 hours to obtain a loaded polyester fiber;
[0011] Step a3: Add the silane coupling agent KH-550 and ethanol solution to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, stir and react for 20-30 minutes at a temperature of 25-30°C and a stirring rate of 300-400r / min, then add the loaded polyester fiber and continue stirring and reacting for 3-5 hours under the condition of heating to reflux. After the reaction, cool the reaction product to room temperature, then vacuum filter, place the filter cake in a vacuum drying oven, and dry it at a temperature of 60-65°C for 6-8 hours to obtain modified polyester fiber.
[0012] As a further solution of the present invention: the usage ratio of the polyester fiber and the sodium hydroxide solution in step a1 is 5g:40-50mL.
[0013] As a further solution of the present invention: the polyester fiber in step a1 is a fully drawn FDY polyester filament fiber with a linear density of 5.41 dtex, and the mass fraction of the sodium hydroxide solution is 10-15%.
[0014] As a further solution of the present invention: the usage ratio of the butyl titanate, silver nitrate, ethanol solution and alkali-treated polyester fiber in step a2 is 5 mL: 0.25-0.55 g: 70-80 mL: 5 g.
[0015] As a further solution of the present invention: the volume fraction of the ethanol solution in step a2 is 30-40%.
[0016] As a further solution of the present invention: the usage ratio of the silane coupling agent KH-550, the ethanol solution and the supported polyester fiber in step a3 is 2.5-5g:90-100mL:10g.
[0017] As a further solution of the present invention: the volume fraction of the ethanol solution in step a3 is 70-80%.
[0018] As a further solution of the present invention: a method for preparing a blended yarn of lyocell fiber and polyester fiber comprises the following steps:
[0019] Step 1: Weigh 50-70 parts of modified polyester fiber and 30-50 parts of lyocell fiber according to weight and set aside;
[0020] Step 2: blending the modified polyester fiber and the lyocell fiber to obtain a blended fiber;
[0021] Step 3: Add the blended fiber into the yarn modification liquid in a mass ratio of 1kg:30-40kg, immerse for 2-3 hours, then take out and drain, then place in a vacuum drying oven, pre-bake at a temperature of 80-85°C for 2-3 minutes, and then bake at a temperature of 110-120°C for 1-2 minutes to obtain a blended yarn of lyocell fiber and polyester fiber.
[0022] As a further solution of the present invention: the yarn modification liquid is prepared by the following steps:
[0023] Step b1: add methyltrifluoropropylcyclotrisiloxane, D4Hcyclotetrasiloxane and tetramethyldisiloxane to a three-necked flask equipped with a stirrer, a thermometer and an air duct, introduce nitrogen protection, stir and react for 25-30 minutes at a temperature of 45-50°C and a stirring rate of 300-400r / min, then add concentrated sulfuric acid and continue to stir and react for 15-20 minutes, then heat to 60-65°C and continue to stir and react for 5-6 hours, after the reaction is completed, cool the reaction product to room temperature, then adjust the pH to 7 with sodium hydroxide solution, then vacuum filter, place the filtrate in a vacuum drying oven, and dry it at 60-65°C for 3-5 hours to obtain intermediate 1;
[0024] Step b2: Add intermediate 1, 2-hydroxyethyl acrylic acid, isopropanol and toluene to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, introduce nitrogen protection, stir and react for 25-30 minutes at a temperature of 25-30° C. and a stirring rate of 300-400 r / min, then add chloroplatinic acid and continue to stir and react for 3-5 minutes, then heat the temperature to 50-55° C. and continue to stir and react for 25-30 minutes, then heat the temperature to 90-95° C. and continue to stir and react for 2-3 hours, after the reaction is completed, cool the reaction product to room temperature, and then remove the solvent by rotary evaporation to obtain intermediate 2;
[0025] Step b3: Add intermediate 2, diphenylmethane diisocyanate, dibutyltin dilaurate and anhydrous acetone to a three-necked flask equipped with an agitator, a thermometer and an air duct, introduce nitrogen protection, stir and react for 2-3 hours at a temperature of 50-55°C and a stirring rate of 300-400r / min, then add N-methyldiethanolamine and continue to stir and react for 8-10 minutes, then heat to 70-75°C and continue to stir and react for 1-1.5 hours, then add methyl ethyl ketone oxime and continue to stir and react for 30-50 minutes, then add decane bromide and continue to stir and react for 2-3 hours, after the reaction is completed, cool the reaction product to room temperature, then rotary evaporate to remove the solvent, then add sodium dodecylbenzene sulfonate and deionized water for shear emulsification for 30-50 minutes to obtain a yarn modified liquid with a solid content of 3-6%.
[0026] As a further solution of the present invention: the usage ratio of the methyltrifluoropropylcyclotrisiloxane, D4Hcyclotetrasiloxane, tetramethyldisiloxane and concentrated sulfuric acid in step b1 is 20-30g: 8-12g: 5-9g: 1.1-1.7g.
[0027] As a further solution of the present invention: the mass fraction of the concentrated sulfuric acid in step b1 is 98%, and the mass fraction of the sodium hydroxide solution is 25-30%.
[0028] As a further scheme of the present invention: the usage ratio of the intermediate 1, 2-hydroxyethyl acrylate, isopropanol, toluene and chloroplatinic acid in step b2 is 30g:1.8-4.6g:30-40mL:50-60mL:0.2-0.4g.
[0029] As a further scheme of the present invention: the usage ratio of the intermediate 2, diphenylmethane diisocyanate, dibutyltin dilaurate, anhydrous acetone, N-methyldiethanolamine, methyl ethyl ketoxime, n-decane bromide and sodium dodecylbenzenesulfonate in step b3 is 20-25g: 6-12g: 0.01-0.03g: 70-80mL: 1.3-2.5g: 0.8-1.4g: 1.5-2.5g: 0.05-0.07g.
[0030] As a further solution of the present invention: an application of the blended yarn of lyocell fiber and polyester fiber in the preparation of denim fabric.
[0031] Beneficial effects of the present invention:
[0032] The invention discloses a lyocell fiber and polyester fiber blended yarn and a preparation method and application thereof. The blended fiber is obtained by blending modified polyester fiber and lyocell fiber, and the blended fiber is added into a yarn modification liquid for immersion, then taken out for draining, and then dried to obtain the lyocell fiber and polyester fiber blended yarn. The preparation method gives full play to the advantages of the modified polyester fiber and the lyocell fiber by reasonably modifying the ratio of the polyester fiber and the lyocell fiber, so that the prepared blended yarn has excellent performance in terms of moisture absorption, air permeability, shape retention, wear resistance, antistatic property and antibacterial property, and has excellent comprehensive performance. The blended yarn is suitable for producing fashionable and environmentally friendly denim fabrics, can improve the quality and functionality of the denim fabrics, and meet people's demand for high-quality denim fabrics. The method has broad market application prospects.
[0033] In the process of preparing lyocell fiber and polyester fiber blended yarn, a modified polyester fiber is first prepared. First, the polyester fiber is placed in a sodium hydroxide solution for alkali treatment to obtain an alkali-treated polyester fiber. After the alkali treatment, the surface layer of the polyester fiber is dissolved and falls off, the surface becomes rough, and many irregularly shaped pits are formed on the surface, so that the specific surface area of the polyester fiber is increased. At the same time, due to the occurrence of the hydrolysis reaction, the polar groups on the surface of the polyester fiber will also increase, which is convenient for the subsequent nanoparticle loading. Then, butyl titanate and silver nitrate are used as raw materials, and the alkali-treated polyester fiber is immersed and then subjected to a hydrothermal reaction, so that nano-titanium dioxide doped with silver ions is loaded on the fiber surface of the alkali-treated polyester fiber to obtain a loaded polyester fiber. Finally, the loaded polyester fiber is modified using a silane coupling agent KH-550. The silane coupling agent KH-55 0 after hydrolysis, the siloxane on it is hydrolyzed to form silanol connected to the fiber surface of the loaded polyester fiber, which is then wrapped with organic matter, and a large amount of amino groups are introduced to obtain modified polyester fiber; the polyester fiber has a high modulus and good elasticity, so that the blended yarn is crisp and wrinkle-resistant, and the prepared denim fabric is not easy to produce creases and deformation during wearing, which can keep a good appearance, and then nano-titanium dioxide is loaded on it. Titanium dioxide, as a photocatalyst, can efficiently decompose bacteria adsorbed on the surface under ultraviolet irradiation, and the bacteria are eliminated in this process, and after being doped with silver ions, the growth and reproduction of bacteria on it can be further inhibited, so that the blended yarn has a long-lasting and broad-spectrum antibacterial function, and the loading of nano-titanium dioxide can improve the surface mechanical strength of the polyester fiber and the wear resistance of the blended yarn, so that the anti-pilling performance of the denim fabric prepared by it is greatly improved;
[0034] In the process of preparing the blended yarn of lyocell fiber and polyester fiber, a yarn modification liquid is also prepared. First, methyl trifluoropropyl cyclotrisiloxane, D4H cyclotetrasiloxane and tetramethyl disiloxane are used as raw materials for polymerization to form terminal hydrogen-containing fluorinated polysiloxane to obtain intermediate 1. Then, intermediate 1 and 2-hydroxyethyl acrylate are reacted, and Si-H on intermediate 1 reacts with the alkenyl on 2-hydroxyethyl acrylate to introduce hydroxyl groups to obtain intermediate 2. Then, intermediate 2 is used as a polyol and diphenylmethane diisocyanate is used as an isocyanate monomer for polymerization. Then, N-methyldiethanolamine is used as a chain extender, and a large number of tertiary amine groups are introduced at the same time. Then, methyl ethyl ketoxime is used for end-capping, and then decane bromide is added for reaction to convert the tertiary amine group into a quaternary ammonium group. Finally, Emulsification is performed to form a yarn modification liquid; the effective ingredients in the yarn modification liquid are polyurethane containing organic silicon, organic fluorine, quaternary ammonium groups and blocked polyurethane, and the isocyanate groups in the polyurethane after the blended fiber is modified react with the highly active hydroxyl and amino groups on the blended fiber to form ester bonds and amide bonds, thereby achieving an anti-wrinkle effect, and at the same time, the introduced organic silicon makes the denim fabric softer and more comfortable to the touch, and at the same time, the presence of organic silicon and organic fluorine can give the denim fabric low surface energy characteristics, can reduce the attachment of dust and stains, and at the same time improve the antistatic performance and lubricity of the fabric, and significantly improve its anti-pilling performance, and the introduced quaternary ammonium group is positively charged and can be adsorbed on the negatively charged cell membrane, causing bacterial cell membrane damage, thereby achieving an antibacterial effect, and can further enhance the antibacterial performance of the blended yarn.
[0035] In summary, the blended yarn and preparation method of the present invention not only bring consumers a more comfortable wearing experience by comprehensively improving the stain resistance, anti-pilling performance and antibacterial performance of denim fabrics, but also can improve the quality and functionality of denim fabrics, meet people's demand for high-quality denim fabrics, and are expected to have a positive role in promoting the textile industry and health protection fields. DETAILED DESCRIPTION
[0036] 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 creative work are within the scope of protection of the present invention.
[0037] Embodiment 1:
[0038] This embodiment is a method for preparing a blended yarn of lyocell fiber and polyester fiber, comprising the following steps:
[0039] Step S1: 5 g of fully stretched FDY polyester filament fiber with a linear density of 5.41 dtex and a sodium hydroxide solution with a mass fraction of 10% are added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at a temperature of 25° C. and a stirring rate of 300 r / min for 20 minutes, and then the temperature is raised to 65° C. and the stirring reaction is continued for 1 hour. After the reaction is completed, the reaction product is cooled to room temperature, and then vacuum filtered, and the filter cake is washed twice with distilled water, and then placed in a vacuum drying oven and dried at a temperature of 50° C. for 2 hours to obtain alkali-treated polyester fiber;
[0040] Step S2: 5 mL of butyl titanate, 0.25 g of silver nitrate and 70 mL of 30% ethanol solution by volume were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction at a temperature of 25° C. and a stirring rate of 300 r / min for 20 min, then 5 g of alkali-treated polyester fiber was added and the temperature was raised to reflux and the stirring reaction was continued for 3 h. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed three times with anhydrous ethanol, anhydrous acetone and distilled water in sequence, and then placed in a vacuum drying oven and dried at a temperature of 60° C. for 4 h to obtain a loaded polyester fiber;
[0041] Step S3: 2.5 g of silane coupling agent KH-550 and 90 mL of 70% ethanol solution by volume were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction at a temperature of 25° C. and a stirring rate of 300 r / min for 20 min, then 10 g of loaded polyester fiber was added and the temperature was raised to reflux and the stirring reaction was continued for 3 h. After the reaction was completed, the reaction product was cooled to room temperature, and then vacuum filtered, and the filter cake was placed in a vacuum drying oven and dried at a temperature of 60° C. for 6 h to obtain modified polyester fiber;
[0042] Step S4: 20 g of methyltrifluoropropylcyclotrisiloxane, 8 g of D4Hcyclotetrasiloxane and 5 g of tetramethyldisiloxane were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred for reaction at a temperature of 45° C. and a stirring rate of 300 r / min for 25 min, and then 1.1 g of 98% concentrated sulfuric acid was added and the stirring reaction was continued for 15 min. The mixture was then heated to 60° C. and the stirring reaction was continued for 5 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the pH value was adjusted to 7 with a 25% sodium hydroxide solution. The mixture was then vacuum filtered, and the filtrate was placed in a vacuum drying oven and dried at 60° C. for 3 h to obtain an intermediate 1.
[0043] Step S5: 30 g of intermediate 1, 1.8 g of 2-hydroxyethyl acrylic acid ester, 30 mL of isopropanol and 50 mL of toluene were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred for reaction at 25° C. and a stirring rate of 300 r / min for 25 min, and then 0.2 g of chloroplatinic acid was added and the stirring reaction was continued for 3 min. The mixture was heated to 50° C. and the stirring reaction was continued for 25 min. The mixture was heated to 90° C. and the stirring reaction was continued for 2 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 2;
[0044] Step S6: 20g of intermediate 2, 6g of diphenylmethane diisocyanate, 0.01g of dibutyltin dilaurate and 70mL of anhydrous acetone are added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen is introduced for protection. The mixture is stirred and reacted for 2h at a temperature of 50°C and a stirring rate of 300r / min, and then 1.3g of N-methyldiethanolamine is added and the stirring reaction is continued for 8min. The mixture is then heated to 70°C and the stirring reaction is continued for 1h. Then, 0.8g of methyl ethyl ketoxime is added and the stirring reaction is continued for 30min. Then, 1.5g of bromodecane is added and the stirring reaction is continued for 2h. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation. Then, 0.05g of sodium dodecylbenzenesulfonate and deionized water are added and sheared and emulsified for 30min to obtain a yarn modified liquid with a solid content of 3%;
[0045] Step S7: weighing 50 parts of modified polyester fiber and 30 parts of lyocell fiber according to weight parts for later use;
[0046] Step S8: blending the modified polyester fiber and the lyocell fiber to obtain a blended fiber;
[0047] Step S9: Add the blended fiber into the yarn modification liquid at a mass ratio of 1kg:30kg and immerse it for 2 hours, then take it out and drain it, then place it in a vacuum drying oven, pre-bake it at 80°C for 2 minutes, and then bake it at 110°C for 1 minute to obtain a blended yarn of lyocell fiber and polyester fiber.
[0048] Embodiment 2:
[0049] This embodiment is a method for preparing a blended yarn of lyocell fiber and polyester fiber, comprising the following steps:
[0050] Step S1: 5 g of fully stretched FDY polyester filament fiber with a linear density of 5.41 dtex and a sodium hydroxide solution with a mass fraction of 12% are added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at a temperature of 28° C. and a stirring rate of 350 r / min for 25 min, and then the temperature is raised to 70° C. and the stirring reaction is continued for 1 h. After the reaction is completed, the reaction product is cooled to room temperature, and then vacuum filtered, and the filter cake is washed twice with distilled water, and then placed in a vacuum drying oven and dried at a temperature of 52° C. for 2.5 h to obtain alkali-treated polyester fiber;
[0051] Step S2: 5 mL of butyl titanate, 0.4 g of silver nitrate and 75 mL of 35% ethanol solution were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction for 25 min at a temperature of 28° C. and a stirring rate of 350 r / min, then 5 g of alkali-treated polyester fiber was added and the temperature was raised to reflux and the stirring reaction was continued for 4 h. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed with anhydrous ethanol, anhydrous acetone and distilled water for 4 times in sequence, and then placed in a vacuum drying oven and dried at a temperature of 62° C. for 4.5 h to obtain a loaded polyester fiber;
[0052] Step S3: adding 3.5 g of silane coupling agent KH-550 and 95 mL of 75% ethanol solution to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, stirring and reacting for 25 min at a temperature of 28° C. and a stirring rate of 350 r / min, then adding 10 g of loaded polyester fiber and heating to reflux and continuing to stir and react for 4 h. After the reaction is completed, the reaction product is cooled to room temperature, then vacuum filtered, and the filter cake is placed in a vacuum drying oven and dried at a temperature of 62° C. for 7 h to obtain modified polyester fiber;
[0053] Step S4: 25 g of methyltrifluoropropylcyclotrisiloxane, 10 g of D4Hcyclotetrasiloxane and 7 g of tetramethyldisiloxane were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred at 48° C. and a stirring rate of 350 r / min for 28 min, and then 1.4 g of 98% concentrated sulfuric acid was added and the stirring reaction was continued for 18 min. The mixture was then heated to 62° C. and the stirring reaction was continued for 5.5 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the pH value was adjusted to 7 with a 28% sodium hydroxide solution. The mixture was then vacuum filtered, and the filtrate was placed in a vacuum drying oven and dried at 62° C. for 4 h to obtain an intermediate 1.
[0054] Step S5: 30 g of intermediate 1, 3.2 g of 2-hydroxyethyl acrylic acid ester, 35 mL of isopropanol and 55 mL of toluene were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred at 28° C. and a stirring rate of 350 r / min for 28 min, and then 0.3 g of chloroplatinic acid was added and the stirring reaction was continued for 4 min. The mixture was heated to 52° C. and the stirring reaction was continued for 28 min. The mixture was heated to 92° C. and the stirring reaction was continued for 2.5 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 2;
[0055] Step S6: 22g of intermediate 2, 9g of diphenylmethane diisocyanate, 0.02g of dibutyltin dilaurate and 75mL of anhydrous acetone were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred and reacted for 2.5h at a temperature of 52°C and a stirring rate of 350r / min. Then, 1.9g of N-methyldiethanolamine was added and the stirring reaction was continued for 9min. Then, the temperature was raised to 72°C and the stirring reaction was continued for 1h. Then, 1.1g of methyl ethyl ketoxime was added and the stirring reaction was continued for 40min. Then, 2.0g of bromodecane was added and the stirring reaction was continued for 2.5h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. Then, 0.06g of sodium dodecylbenzene sulfonate and deionized water were added and sheared and emulsified for 40min to obtain a yarn modified liquid with a solid content of 4.5%;
[0056] Step S7: weighing 60 parts of modified polyester fiber and 40 parts of lyocell fiber according to weight parts for later use;
[0057] Step S8: blending the modified polyester fiber and the lyocell fiber to obtain a blended fiber;
[0058] Step S9: Add the blended fiber to the yarn modification liquid at a mass ratio of 1kg:35kg and immerse it for 2.5 hours. Then take it out and drain it. Then place it in a vacuum drying oven, pre-bake it at 82°C for 2.5 minutes, and then bake it at 115°C for 1.5 minutes to obtain a blended yarn of lyocell fiber and polyester fiber.
[0059] Embodiment 3:
[0060] This embodiment is a method for preparing a blended yarn of lyocell fiber and polyester fiber, comprising the following steps:
[0061] Step S1: 5 g of fully stretched FDY polyester filament fiber with a linear density of 5.41 dtex and a sodium hydroxide solution with a mass fraction of 15% are added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at a temperature of 30° C. and a stirring rate of 400 r / min for 30 min, and then the temperature is raised to 75° C. and the stirring reaction is continued for 1.5 h. After the reaction is completed, the reaction product is cooled to room temperature, and then vacuum filtered, and the filter cake is washed with distilled water for 3 times, and then placed in a vacuum drying oven and dried at a temperature of 55° C. for 3 h to obtain alkali-treated polyester fiber;
[0062] Step S2: 5 mL of butyl titanate, 0.55 g of silver nitrate and 80 mL of 40% ethanol solution by volume were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction at a temperature of 30° C. and a stirring rate of 400 r / min for 30 min, then 5 g of alkali-treated polyester fiber was added and the temperature was raised to reflux and the stirring reaction was continued for 5 h. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed with anhydrous ethanol, anhydrous acetone and distilled water for 5 times in sequence, and then placed in a vacuum drying oven and dried at a temperature of 65° C. for 5 h to obtain a loaded polyester fiber;
[0063] Step S3: 5 g of silane coupling agent KH-550 and 100 mL of 80% ethanol solution by volume were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction at a temperature of 30° C. and a stirring rate of 400 r / min for 30 min, then 10 g of loaded polyester fiber was added and the temperature was raised to reflux and the stirring reaction was continued for 5 h. After the reaction was completed, the reaction product was cooled to room temperature, and then vacuum filtered, and the filter cake was placed in a vacuum drying oven and dried at a temperature of 65° C. for 8 h to obtain modified polyester fiber;
[0064] Step S4: 30 g of methyltrifluoropropylcyclotrisiloxane, 12 g of D4Hcyclotetrasiloxane and 9 g of tetramethyldisiloxane were added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen was introduced for protection. The mixture was stirred at 50° C. and a stirring rate of 400 r / min for 30 min, and then 1.7 g of 98% concentrated sulfuric acid was added and the stirring reaction was continued for 20 min. The mixture was then heated to 65° C. and the stirring reaction was continued for 6 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the pH value was adjusted to 7 with a 30% sodium hydroxide solution. The mixture was then vacuum filtered, and the filtrate was placed in a vacuum drying oven and dried at 65° C. for 5 h to obtain an intermediate 1.
[0065] Step S5: 30 g of intermediate 1, 4.6 g of 2-hydroxyethyl acrylic acid ester, 40 mL of isopropanol and 60 mL of toluene were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred for reaction at a temperature of 30° C. and a stirring rate of 400 r / min for 30 min, and then 0.4 g of chloroplatinic acid was added and the stirring reaction was continued for 5 min. The mixture was heated to 55° C. and the stirring reaction was continued for 30 min. The mixture was heated to 95° C. and the stirring reaction was continued for 3 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 2;
[0066] Step S6: 25g of intermediate 2, 12g of diphenylmethane diisocyanate, 0.03g of dibutyltin dilaurate and 80mL of anhydrous acetone were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred and reacted for 3h at a temperature of 55°C and a stirring rate of 400r / min, and then 2.5g of N-methyldiethanolamine was added and the stirring reaction was continued for 10min. The mixture was heated to 75°C and the stirring reaction was continued for 1.5h. Then 1.4g of methyl ethyl ketoxime was added and the stirring reaction was continued for 50min. Then 2.5g of bromodecane was added and the stirring reaction was continued for 3h. After the reaction was completed, the reaction product was cooled to room temperature, and the solvent was removed by rotary evaporation. Then 0.07g of sodium dodecylbenzenesulfonate and deionized water were added and sheared and emulsified for 50min to obtain a yarn modified liquid with a solid content of 6%;
[0067] Step S7: weighing 70 parts of modified polyester fiber and 50 parts of lyocell fiber according to weight parts for later use;
[0068] Step S8: blending the modified polyester fiber and the lyocell fiber to obtain a blended fiber;
[0069] Step S9: Add the blended fiber into the yarn modification liquid at a mass ratio of 1kg:40kg and immerse for 3 hours, then take out and drain, then place in a vacuum drying oven, pre-bake at 85°C for 3 minutes, and then bake at 120°C for 2 minutes to obtain a blended yarn of lyocell fiber and polyester fiber.
[0070] Comparative Example 1:
[0071] This comparative example is a method for preparing a blended yarn of lyocell fiber and polyester fiber, comprising the following steps:
[0072] Step S1: weigh 70 parts of 5g fully stretched FDY polyester filament fiber with a linear density of 5.41dtex and 50 parts of lyocell fiber according to weight, and set aside;
[0073] Step S2: 5 g of fully drawn FDY polyester filament fiber with a linear density of 5.41 dtex and lyocell fiber are blended to obtain a blended yarn of lyocell fiber and polyester fiber.
[0074] Comparative Example 2:
[0075] This comparative example is a method for preparing a blended yarn of lyocell fiber and polyester fiber, comprising the following steps:
[0076] Step S1: 5 g of fully stretched FDY polyester filament fiber with a linear density of 5.41 dtex and a sodium hydroxide solution with a mass fraction of 15% are added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at a temperature of 30° C. and a stirring rate of 400 r / min for 30 min, and then the temperature is raised to 75° C. and the stirring reaction is continued for 1.5 h. After the reaction is completed, the reaction product is cooled to room temperature, and then vacuum filtered, and the filter cake is washed with distilled water for 3 times, and then placed in a vacuum drying oven and dried at a temperature of 55° C. for 3 h to obtain alkali-treated polyester fiber;
[0077] Step S2: 5 mL of butyl titanate, 0.55 g of silver nitrate and 80 mL of 40% ethanol solution by volume were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction at a temperature of 30° C. and a stirring rate of 400 r / min for 30 min, then 5 g of alkali-treated polyester fiber was added and the temperature was raised to reflux and the stirring reaction was continued for 5 h. After the reaction was completed, the reaction product was cooled to room temperature and then vacuum filtered. The filter cake was washed with anhydrous ethanol, anhydrous acetone and distilled water for 5 times in sequence, and then placed in a vacuum drying oven and dried at a temperature of 65° C. for 5 h to obtain a loaded polyester fiber;
[0078] Step S3: 5 g of silane coupling agent KH-550 and 100 mL of 80% ethanol solution by volume were added to a three-necked flask equipped with a stirrer, a thermometer and a reflux condenser, and stirred for reaction at a temperature of 30° C. and a stirring rate of 400 r / min for 30 min, then 10 g of loaded polyester fiber was added and the temperature was raised to reflux and the stirring reaction was continued for 5 h. After the reaction was completed, the reaction product was cooled to room temperature, and then vacuum filtered, and the filter cake was placed in a vacuum drying oven and dried at a temperature of 65° C. for 8 h to obtain modified polyester fiber;
[0079] Step S4: weighing 70 parts of modified polyester fiber and 50 parts of lyocell fiber according to weight parts for later use;
[0080] Step S5: blending the modified polyester fiber and the lyocell fiber to obtain a blended yarn of the lyocell fiber and the polyester fiber.
[0081] Comparative Example 3:
[0082] This comparative example is a method for preparing a blended yarn of lyocell fiber and polyester fiber, comprising the following steps:
[0083] Step S1: 30 g of methyltrifluoropropylcyclotrisiloxane, 12 g of D4Hcyclotetrasiloxane and 9 g of tetramethyldisiloxane are added to a three-necked flask equipped with a stirrer, a thermometer and an air duct, and nitrogen is introduced for protection. The mixture is stirred and reacted for 30 min at a temperature of 50° C. and a stirring rate of 400 r / min. Then, 1.7 g of 98% concentrated sulfuric acid is added and the stirring reaction is continued for 20 min. Then, the mixture is heated to 65° C. and the stirring reaction is continued for 6 h. After the reaction is completed, the reaction product is cooled to room temperature, and then the pH value is adjusted to 7 with a 30% sodium hydroxide solution. Then, the mixture is vacuum filtered, and the filtrate is placed in a vacuum drying oven and dried at 65° C. for 5 h to obtain an intermediate 1.
[0084] Step S2: 30 g of intermediate 1, 4.6 g of 2-hydroxyethyl acrylic acid ester, 40 mL of isopropanol and 60 mL of toluene were added to a three-necked flask equipped with a stirrer, a thermometer and a gas duct, and nitrogen was introduced for protection. The mixture was stirred for reaction at 30° C. and a stirring rate of 400 r / min for 30 min, and then 0.4 g of chloroplatinic acid was added and the stirring reaction was continued for 5 min. The mixture was heated to 55° C. and the stirring reaction was continued for 30 min. The mixture was heated to 95° C. and the stirring reaction was continued for 3 h. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain intermediate 2;
[0085] Step S3: 25g of intermediate 2, 12g of diphenylmethane diisocyanate, 0.03g of dibutyltin dilaurate and 80mL of anhydrous acetone are added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen is introduced for protection. The mixture is stirred and reacted for 3h at a temperature of 55°C and a stirring rate of 400r / min, and then 2.5g of N-methyldiethanolamine is added and the stirring reaction is continued for 10min. The mixture is then heated to 75°C and the stirring reaction is continued for 1.5h. Then 1.4g of methyl ethyl ketoxime is added and the stirring reaction is continued for 50min. Then 2.5g of bromodecane is added and the stirring reaction is continued for 3h. After the reaction is completed, the reaction product is cooled to room temperature, and the solvent is removed by rotary evaporation. Then 0.07g of sodium dodecylbenzenesulfonate and deionized water are added and sheared and emulsified for 50min to obtain a yarn modified liquid with a solid content of 6%;
[0086] Step S4: 70 parts of fully stretched FDY polyester filament fiber with a linear density of 5.41 dtex and 50 parts of lyocell fiber are weighed according to weight and set aside;
[0087] Step S5: blending the fully stretched FDY polyester filament fiber with a linear density of 5.41 dtex and the lyocell fiber to obtain a blended fiber;
[0088] Step S6: Add the blended fiber into the yarn modification liquid at a mass ratio of 1kg:40kg and immerse for 3 hours, then take it out and drain it, then place it in a vacuum drying oven, pre-bake it at 85°C for 3 minutes, and then bake it at 120°C for 2 minutes to obtain a blended yarn of lyocell fiber and polyester fiber.
[0089] Performance Test:
[0090] The lyocell fiber and polyester fiber blended yarn of Examples 1-3 and Comparative Examples 1-3 were used as weft yarns and cotton yarns were used as warp yarns to interweave to obtain denim fabrics, and the weft density of the denim fabrics was 280 yarns / 10 cm, the warp density was 300 yarns / 10 cm, and the surface density was 700 g / m 2 ;
[0091] The denim fabric was quantitatively tested for antibacterial properties according to GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method", and the antibacterial properties of each fabric after 50 washes were compared. The fabrics were evaluated for pilling grade after friction in a rating box using incandescent fluorescent tubes according to GB / T4802.2-2008 "Determination of pilling properties of textile fabrics Part 2: Modified Martindale method";
[0092] The test results are shown in Table 1:
[0093] Table 1 Evaluation results of antibacterial performance and anti-pilling performance
[0094]
[0095] Referring to the data in Table 1, based on the comparison between Examples 1-3 and Comparative Examples 1-3, it can be seen that the use of modified polyester fibers for blending and modification using yarn modification liquid can significantly improve the antibacterial properties of lyocell fiber and polyester fiber blended yarns, and the anti-pilling performance of the denim fabrics prepared thereby is greatly improved.
[0096] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0097] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined in this application, they shall all fall within the protection scope of the present invention.
Claims
1. A method for preparing a blended yarn of lyocell fiber and polyester fiber, characterized in that: The following steps are involved: Step 1: Weigh 50-70 parts of modified polyester fiber and 30-50 parts of lyocell fiber according to weight and set aside; Step 2: blending the modified polyester fiber and the lyocell fiber to obtain a blended fiber; Step 3: adding the blended fiber to the yarn modification liquid at a mass ratio of 1kg:30-40kg and immersing for 2-3h, then taking it out and draining it, and then placing it in a vacuum drying oven, pre-baking it at a temperature of 80-85°C for 2-3min, and then baking it at a temperature of 110-120°C for 1-2min, to obtain a blended yarn of lyocell fiber and polyester fiber; Wherein, the modified polyester fiber is prepared by the following steps: Step a1: stirring the polyester fiber and the sodium hydroxide solution to react, cooling the reaction product after the reaction is completed, and then vacuum filtering, washing and drying the filter cake to obtain the alkali-treated polyester fiber; Step a2: stirring butyl titanate, silver nitrate and ethanol solution for reaction, then adding alkali-treated polyester fiber and continuing stirring for reaction, cooling the reaction product after the reaction is completed, then vacuum filtering, washing and drying the filter cake to obtain loaded polyester fiber; Step a3: Stirring the silane coupling agent KH-550 and the ethanol solution for reaction, then adding the supported polyester fiber and continuing the stirring reaction, cooling the reaction product after the reaction is completed, then vacuum filtering, and drying the filter cake to obtain the modified polyester fiber; Wherein, the yarn modification liquid is prepared by the following steps: Step b1: stirring methyltrifluoropropylcyclotrisiloxane, D4Hcyclotetrasiloxane and tetramethyldisiloxane for reaction, then adding concentrated sulfuric acid and continuing stirring for reaction, cooling the reaction product after the reaction is completed, then adjusting the pH with sodium hydroxide solution, then vacuum filtering, and drying the filtrate to obtain intermediate 1; Step b2: stirring the intermediate 1, 2-hydroxyethyl acrylate, isopropanol and toluene for reaction, then adding chloroplatinic acid and continuing the stirring reaction, cooling the reaction product after the reaction is completed, and then rotary evaporating to obtain the intermediate 2; Step b3: Stir the intermediate 2, diphenylmethane diisocyanate, dibutyltin dilaurate and anhydrous acetone for reaction, then add N-methyldiethanolamine, methyl ethyl ketoxime and decane bromide in sequence and continue stirring the reaction. After the reaction is completed, cool the reaction product, then rotary evaporate, and then add sodium dodecylbenzene sulfonate and deionized water for shear emulsification to obtain a yarn modified liquid.
2. The method for preparing a blended yarn of lyocell fiber and polyester fiber according to claim 1, characterized in that: The dosage ratio of the polyester fiber and the sodium hydroxide solution in step a1 is 5g:40-50mL; the mass fraction of the sodium hydroxide solution is 10-15%.
3. The method for preparing a lyocell fiber and polyester fiber blended yarn according to claim 1, characterized in that: The usage ratio of the butyl titanate, silver nitrate, ethanol solution and alkali-treated polyester fiber in step a2 is 5 mL: 0.25-0.55 g: 70-80 mL: 5 g; the volume fraction of the ethanol solution is 30-40%.
4. The method for preparing a lyocell fiber and polyester fiber blended yarn according to claim 1, characterized in that: The usage ratio of the silane coupling agent KH-550, ethanol solution and supported polyester fiber in step a3 is 2.5-5g:90-100mL:10g; The volume fraction of the ethanol solution is 70-80%.
5. The method for preparing a blended yarn of lyocell fiber and polyester fiber according to claim 1, characterized in that: The usage ratio of the methyltrifluoropropylcyclotrisiloxane, D4Hcyclotetrasiloxane, tetramethyldisiloxane and concentrated sulfuric acid in step b1 is 20-30g: 8-12g: 5-9g: 1.1-1.7g; the mass fraction of the concentrated sulfuric acid is 98%, and the mass fraction of the sodium hydroxide solution is 25-30%.
6. The method for preparing a blended yarn of lyocell fiber and polyester fiber according to claim 1, characterized in that: The usage ratio of the intermediate 1, 2-hydroxyethyl acrylate, isopropanol, toluene and chloroplatinic acid in step b2 is 30g:1.8-4.6g:30-40mL:50-60mL:0.2-0.4g.
7. The method for preparing a blended yarn of lyocell fiber and polyester fiber according to claim 1, characterized in that: The amount ratio of the intermediate 2, diphenylmethane diisocyanate, dibutyltin dilaurate, anhydrous acetone, N-methyldiethanolamine, methyl ethyl ketoxime, n-decane bromide and sodium dodecylbenzenesulfonate in step b3 is 20-25g: 6-12g: 0.01-0.03g: 70-80mL: 1.3-2.5g: 0.8-1.4g: 1.5-2.5g: 0.05-0.07g.
8. A blended yarn of lyocell fiber and polyester fiber, characterized in that: The lyocell fiber and polyester fiber blended yarn is prepared according to the preparation method of the lyocell fiber and polyester fiber blended yarn according to any one of claims 1-7.
9. Use of the blended yarn of lyocell fiber and polyester fiber according to claim 8 in preparing denim fabrics.
Citation Information
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Polysiloxane modified polyester fiber as well as preparation method and application thereof
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