Moisture-absorbing antibacterial functional composite textile fiber and preparation method thereof
The preparation of composite microcapsules through NaOH solution pretreatment and high-speed shear emulsification technology has solved the problem of poor hygroscopicity and antibacteriality of pure cotton yarns, achieved efficient hygroscopicity and antibacterial performance of fibers, formed stable composite microcapsules, and improved the Wet conduction properties of fibers.
Patent Information
- Application Number
- CN202411307389.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-09-19
- Publication Date
- 2025-01-10
AI Technical Summary
Pure cotton yarns have poor hygroscopicity and antibacterial properties under hot and humid conditions, and the existing microcapsule preparation process fails to effectively control the stability and particle size uniformity of composite microcapsules, affecting the moisture-absorbing and sweating function and antibacterial properties of textiles.
Pretreat pure cotton yarn with NaOH solution, and mix vinylidene fluoride, acrylic acid, methyl methacrylate and other monomers through a high-speed shear emulsifier, combine inorganic nanoparticles and antibacterial dispersants to prepare composite microcapsules, through low-voltage The concentration of alkali liquid and aqueous phase system adjusts the pH value to form stable composite microcapsules, enhancing the hygroscopic and antibacterial properties of the fiber.
It improves the hygroscopicity and antibacterial properties of textile fibers, enhances the modification degree and antibacterial effect of fibers, has excellent antibacterial effects on Gram-positive and negative bacteria, and improves the moisture-conducting properties of fibers.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of textile materials, and in particular to a moisture-absorbing and antibacterial functional composite textile fiber and a preparation method thereof. Background Art
[0002] Pure cotton yarn is composed of cotton fibers, which are soft, comfortable, skin-friendly and breathable. However, under hot and humid conditions, pure cotton fabrics have slow moisture conduction and release rates due to the moisture absorption, swelling and deformation of the fibers and the moisture storage themselves. This greatly reduces the moisture absorption and perspiration function of pure cotton fabrics, affects the moisture and heat exchange between human skin and the outside world, and makes the human body feel stuffy. In addition, cotton fibers are prone to breed bacteria, fungi and other microorganisms. Under suitable external conditions, microorganisms will multiply rapidly and spread diseases through contact. How to improve the antibacterial properties of cotton fabrics is also a technical problem that needs to be solved urgently.
[0003] In the process of modifying pure cotton yarn, the modified material is microencapsulated, which can not only improve the usability of the material, but also improve the efficiency of the use of the material. Microcapsule technology includes the preparation technology and application technology of microcapsules. It adopts specific methods and specific equipment to use film-forming materials to encapsulate solids, liquids or gases to form tiny particles, which are then mixed with other materials and applied to the fiber fabric to be used. Without destroying the wrapping film, the wrapped object can be diffused through the wrapping film and released outward, resulting in controlled release performance. Microcapsule technology can not only improve the performance of the material, but also improve the efficiency of the material.
[0004] When preparing microcapsules, dispersants and their concentrations are important factors in determining the average particle size and particle size distribution of microcapsule particles. The molecular structure of the dispersant contains both lipophilic and hydrophilic groups. Relying on its amphiphilicity, it can evenly disperse inorganic particles that cannot disperse themselves into the medium in the solvent. The polymer dispersant's high molecular structure contains polar groups such as carboxyl and amino groups. These groups are mainly adsorbed to the surface of inorganic particles through ionic bonds, hydrogen bonds, and intermolecular forces. How to improve the dispersant and thereby improve the stability of the prepared composite microcapsules and control the average particle size of the prepared composite microcapsules is also a technical problem that needs to be solved urgently.
[0005] Patent application CN104178880A discloses a plant antibacterial, skin-beautifying functional health care home textile fabric and its preparation method. The warp yarn is siro-spun yarn, and evening primrose oil with plant antibacterial ingredients is in the form of microcapsules and arranged in the home textile fabric through a padding process to exert antibacterial effects; however, the above-mentioned microcapsule preparation process does not take into account improving the stability of the composite microcapsules and the uniformity of the particle size. In addition, how to improve the hygroscopicity of the fabric is also a technical problem that needs to be solved urgently.
[0006] In view of the technical defects in this aspect, a solution is now proposed. Summary of the invention
[0007] The purpose of the present invention is to provide a hygroscopic and antibacterial functional composite textile fiber and a preparation method thereof, which is used to solve the poor hygroscopicity and antibacterial properties of pure cotton yarn in the prior art. When using microcapsules to modify textile fibers, how to control the stability of the microcapsules and the uniformity of the particle size are also technical problems that need to be solved urgently.
[0008] The purpose of the present invention can be achieved by the following technical solution: A method for preparing a hygroscopic and antibacterial functional composite textile fiber, comprising the following steps:
[0009] S1. Soaking pure cotton yarn in NaOH solution, filtering and drying to constant weight to obtain pretreated pure cotton yarn; mixing composite microcapsules and deionized water evenly to obtain functional textile solution;
[0010] The pure cotton yarn is soaked in a low concentration alkali solution to obtain the pretreated pure cotton yarn.
[0011] S2. The pretreated pure cotton yarn and the functional textile liquid are mixed according to a bath ratio of 1:40-50, heated in a water bath, and then filtered out to obtain the modified yarn; the modified yarn is post-processed to obtain a hygroscopic and antibacterial functional fiber.
[0012] Furthermore, the preparation method of the composite microcapsule comprises the following steps:
[0013] A1, vinylidene fluoride, acrylic acid, methyl methacrylate, acetone, a crosslinking agent and an initiator are uniformly mixed to obtain an oil phase;
[0014] Acetone is used as a low boiling point solvent, dicumyl peroxide is used as a crosslinking agent, benzoyl peroxide is used as an initiator, and vinylidene fluoride, acrylic acid and methyl methacrylate are used as monomer components. The above substances are mixed evenly to prepare an oil phase.
[0015] A2, grinding inorganic nanoparticles of zirconium oxide, zinc oxide or titanium dioxide to 100-300 mesh to obtain an inorganic powder material; mixing distilled water, NaCl, inorganic powder material, antibacterial dispersant and octadecyldimethyl[3-(trimethylsilyl)propyl]ammonium chloride to obtain an aqueous phase system; adjusting the pH value of the aqueous phase system to 3-4 with 0.1 mol / L hydrochloric acid solution to obtain an aqueous phase;
[0016] The water phase components prepared by the invention include antibacterial dispersant, distilled water, NaCl which is helpful for preparing microcapsules with uniform particle size, antibacterial quaternary ammonium salt which is easily soluble in water, and antibacterial dispersant which helps oil phase to be evenly distributed and stable in water phase.
[0017] A3. The water phase and the oil phase are added to a high-speed shear emulsifier and pre-dispersed at 1000-2000 r / min for 5-10 minutes to obtain a pre-dispersed system; the pre-dispersed system is polymerized at 60-70° C. for 6-8 hours, and after post-processing, composite microcapsules are obtained.
[0018] Under the action of high-speed shear emulsification, water, dispersants and additives constitute the water phase; polymerization monomers, foaming agents and initiators constitute the oil phase; as the polymerization reaction proceeds, the thickness of the capsule membrane increases until the monomer is exhausted, thus forming a single-core capsule.
[0019] Furthermore, in step A1, the ratio of ethylenediaminetetrafluoroethylene, methyl methacrylate, acetone, crosslinking agent and initiator is 30-40:30-40:10-15:1-3:200:0.5-1 in parts by weight; in step A2, the ratio of distilled water, NaCl, inorganic powder material, antibacterial dispersant, octadecyldimethyl[3-(trimethylsilyl)propyl]ammonium chloride and antioxidant is 50-80:15-25:5-10:2-5:5-10:0.15-2 in parts by weight.
[0020] Furthermore, in step A3, the ratio of the amount of the water phase to the oil phase is 1:1 in parts by weight; the post-process treatment includes: naturally cooling to room temperature to obtain a product; filtering the product, centrifuging and separating the sedimentation to obtain a solid; washing the solid with deionized water, and then vacuum drying at 70-80°C to constant weight to obtain a composite microcapsule.
[0021] Furthermore, the preparation method of the antibacterial dispersant comprises the following steps:
[0022] B1, adipic acid, diethanolamine and hydroxyethyl methacrylate are uniformly mixed to obtain a mixed solid-liquid;
[0023] B2. The mixed solid and liquid are subjected to polycondensation reaction at 140-160° C. for 2-4 hours to obtain a product; the acidity value of the product is measured; when the conversion rate of the polycondensation reaction reaches more than 80%, the reaction is stopped and the reaction is deemed to be completed, thereby obtaining a polycondensation product;
[0024] Adipic acid, diethanolamine and hydroxyethyl methacrylate undergo esterification reaction to obtain a polycondensation product as follows:
[0025]
[0026] B3. Mix the polycondensation product, 2-butene-1,4-diol bis(bromoacetate), initiator BPO and ethanol, and react at 80-90° C. for 2-3 hours under a nitrogen atmosphere to obtain a product; distill the product under reduced pressure at 70-80° C. to remove the ethanol solvent to obtain a solid product; grind the solid product to 200-300 mesh to obtain an antibacterial dispersant.
[0027] Under the action of an initiator, ethanol is used as a reaction solvent, and the polycondensation product and 2-butene-1,4-diol bis(bromoacetate) ester each contain an unsaturated double bond, and then undergo an addition polymerization reaction to prepare an antibacterial dispersant.
[0028] The polycondensation product and 2-butene-1,4-diol bis(bromoacetate) undergo addition polymerization to obtain an antimicrobial dispersant as follows:
[0029]
[0030] The polycondensate prepared by the present invention is a polymer containing a branched chain. First, adipic acid, diethanolamine and hydroxyethyl methacrylate undergo an addition polymerization reaction to form a linear polycondensate. The linear polycondensate contains an unsaturated double bond and can undergo an addition polymerization reaction with 2-butene-1,4-diol bis(bromoacetate) to obtain a polycondensate containing a branched chain, which is the antibacterial dispersant prepared by the present invention.
[0031] Furthermore, in step B1, the amount ratio of adipic acid, diethanolamine, hydroxyethyl methacrylate and toluenesulfonic acid is 15-30g:7-15g:13-18g:0.1-0.3g; in step B3, the amount ratio of the condensation product, 2-butene-1,4-diol bis(bromoacetate), initiator BPO and ethanol is 20-30g:30-40mL:0.5-1g:200mL.
[0032] Furthermore, in step S1, the concentration of the NaOH solution is 10 g / L, and the solid-liquid ratio of the pure cotton yarn and the NaOH solution is 10:1; the immersion temperature is 10°C and the immersion time is 100-120 min; the dosage ratio of the composite microcapsule and deionized water is 5-10 g:200-300 mL; in step S2, the water bath heating temperature is 30-40°C and the water bath heating time is 30 min; the post-process treatment includes washing the modified yarn with deionized water 3 times, and then drying it at 45°C to constant weight.
[0033] As another aspect of the present invention, a method for preparing a hygroscopic and antibacterial functional composite textile fiber prepares the hygroscopic and antibacterial functional composite textile fiber.
[0034] The present invention has the following beneficial effects:
[0035] 1. When pure cotton yarn is treated with functional textile liquid doped with composite microcapsules, it is treated with low-concentration weak alkali liquid in advance to remove wax and pectin contained in the cuticle of cotton fiber. The pure cotton yarn is soaked and boiled with dilute alkali liquid at an appropriate temperature to remove impurities; in addition, the pure cotton yarn treated with alkali liquid has stronger adsorption performance with functional textile liquid, thereby improving its own modification degree. The above-mentioned functional textile liquid is specifically a mixture of composite microcapsules and deionized water. The composite microcapsules are obtained by high-speed emulsification of water phase and oil phase and post-processing; the oil phase includes vinylidene fluoride, acrylic acid, methyl methacrylate and related additives, and vinylidene fluoride, acrylic acid and methyl methacrylate form the wall material of the oil phase; the water phase includes distilled water, inorganic powder material, antibacterial dispersant, octadecyl dimethyl [3- (trimethylsilyl) propyl] ammonium chloride and related additives; wherein the inorganic powder material is specifically any one of inorganic nanoparticles zirconium oxide, zinc oxide or titanium dioxide, and the rough structure constructed by the inorganic particles is conducive to achieving the super hydrophobicity of the fiber. Octadecyl dimethyl [3- (trimethylsilyl) propyl] ammonium chloride can destroy cell walls and cell membranes, and has a broad spectrum of bactericidal properties, which is manifested as excellent bactericidal effects on Gram-positive bacteria, Gram-negative bacteria, etc. The hydrophobic inorganic powder material and octadecyl dimethyl [3- (trimethylsilyl) propyl] ammonium chloride with antibacterial properties are used as core materials to protect them and improve the sustained-release efficacy.
[0036] 2. When preparing composite microcapsules, due to the excessive interfacial tension between the oil phase and the water phase, it is difficult for the water phase and the oil phase to be evenly dispersed during the high-speed emulsification process to form composite microcapsules with uniform particle size and stability. The uniform dispersion of the oil phase monomer droplets in the water phase and the maintenance of its stable dispersion state are the key to completing the polymerization reaction. The antibacterial dispersant can effectively prevent the particles from condensing and precipitating, so that it can maintain dispersibility and suspension stability during the high-speed emulsification process. The antibacterial dispersant prepared by the present invention is a branched dispersant, and its structural configuration can further increase its own adsorption capacity; the imino and bromine atom functional groups in the antibacterial dispersant undergo chemical adsorption or ion exchange on the surface of solid particles of opposite charge to form a double electron layer, thereby further enhancing the dispersion effect. 2-Butene-1.4-diol bis(bromoacetic acid) ester itself has a broad-spectrum bactericidal property, so that the prepared composite microcapsules have antibacterial properties in both the wall material and the wall core. DETAILED DESCRIPTION
[0037] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. 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.
[0038] Example 1
[0039] This embodiment provides a method for preparing an antibacterial dispersant for a hygroscopic and antibacterial functional composite textile fiber, comprising the following steps:
[0040] B1. A 500 mL four-necked flask was equipped with a thermometer, a condenser, a water separator and an agitator. 15 g of adipic acid, 7 g of diethanolamine, 13 g of hydroxyethyl methacrylate and 0.1 g of p-toluenesulfonic acid as a catalyst were added to the four-necked flask. The four-necked flask was transferred to an oil bath and stirred at 100 r / min to obtain a uniformly mixed solid-liquid mixture.
[0041] B2. Seal the four-necked flask, maintain the temperature of the four-necked flask at 140° C., and carry out polycondensation reaction for 2 hours to obtain a product; sample the product, cool the sample to room temperature, and measure its acidity value. When the conversion rate of the above polycondensation reaction reaches more than 80%, stop the reaction, and the reaction is considered to be completed to obtain a polycondensation product.
[0042] B3. 20 g of the polycondensation product, 30 mL of 2-butene-1,4-diol bis(bromoacetate), 0.5 g of initiator BPO and 200 mL of ethanol were mixed and added into a 500 mL three-necked reaction flask, a magnetic stirrer was placed in the three-necked reaction flask, and nitrogen was filled into the flask after vacuumizing it with liquid nitrogen and thawing it. The three-necked reaction flask was then immersed in an oil bath at 80° C., mixed and stirred at 300 r / min, and reacted for 2 h to obtain a product; the product was distilled under reduced pressure at 70° C. to remove the ethanol solvent to obtain a solid product; the solid product was ground to 200 mesh to obtain an antibacterial dispersant.
[0043] Example 2
[0044] This embodiment provides a method for preparing an antibacterial dispersant for a hygroscopic and antibacterial functional composite textile fiber, comprising the following steps:
[0045] B1. A 500 mL four-necked flask was equipped with a thermometer, a condenser, a water separator and an agitator. 20 g of adipic acid, 10 g of diethanolamine, 15 g of hydroxyethyl methacrylate and 0.2 g of p-toluenesulfonic acid as a catalyst were added to the four-necked flask. The four-necked flask was transferred to an oil bath and stirred at 150 r / min to obtain a uniformly mixed solid-liquid mixture.
[0046] B2. Seal the four-necked flask, maintain the temperature of the four-necked flask at 150° C., and carry out polycondensation reaction for 3 hours to obtain a product; sample the product, cool the sample to room temperature, and measure its acidity value. When the conversion rate of the above polycondensation reaction reaches more than 80%, stop the reaction, and the reaction is considered to be completed to obtain a polycondensation product.
[0047] B3. 26 g of the polycondensation product, 35 mL of 2-butene-1,4-diol bis(bromoacetate), 0.6 g of initiator BPO and 200 mL of ethanol were mixed and added into a 500 mL three-necked reaction flask, a magnetic stirrer was placed in the three-necked reaction flask, and the flask was filled with nitrogen after vacuumizing with liquid nitrogen and thawed. The three-necked reaction flask was then immersed in an oil bath at 82° C., mixed and stirred at 330 r / min, and reacted for 2.3 h to obtain a product; the product was distilled under reduced pressure at 75° C. to remove the ethanol solvent to obtain a solid product; the solid product was ground to 250 mesh to obtain an antibacterial dispersant.
[0048] Example 3
[0049] This embodiment provides a method for preparing an antibacterial dispersant for a hygroscopic and antibacterial functional composite textile fiber, comprising the following steps:
[0050] B1. A 500 mL four-necked flask was equipped with a thermometer, a condenser, a water separator and an agitator. 30 g of adipic acid, 15 g of diethanolamine, 18 g of hydroxyethyl methacrylate and 0.3 g of p-toluenesulfonic acid as a catalyst were added to the four-necked flask. The four-necked flask was transferred to an oil bath and mixed and stirred at 200 r / min to obtain a uniformly mixed solid-liquid mixture.
[0051] B2. Seal the four-necked flask, maintain the temperature of the four-necked flask at 160° C., and carry out polycondensation reaction for 4 hours to obtain a product; sample the product, cool the sample to room temperature, and measure its acidity value. When the conversion rate of the above polycondensation reaction reaches more than 80%, stop the reaction, and the reaction is considered to be completed to obtain a polycondensation product.
[0052] B3. 30 g of the polycondensation product, 40 mL of 2-butene-1,4-diol bis(bromoacetate), 1 g of initiator BPO and 200 mL of ethanol were mixed and added into a 500 mL three-necked reaction flask, a magnetic stirrer was placed in the three-necked reaction flask, and the flask was evacuated by freezing with liquid nitrogen and then filled with nitrogen and thawed. The three-necked reaction flask was then immersed in an oil bath at 90° C., mixed and stirred at 400 r / min, and reacted for 3 h to obtain a product; the product was distilled under reduced pressure at 80° C. to remove the ethanol solvent to obtain a solid product; the solid product was ground to 300 mesh to obtain an antibacterial dispersant.
[0053] Example 4
[0054] This embodiment provides a method for preparing a composite microcapsule for a hygroscopic and antibacterial functional composite textile fiber, comprising the following steps:
[0055] A1. According to parts by weight, 30 parts of vinylidene fluoride, 30 parts of acrylic acid, 10 parts of methyl methacrylate, 1 g of a cross-linking agent, 200 parts of acetone and 0.5 parts of an initiator are mixed uniformly to obtain an oil phase.
[0056] A2, inorganic nanoparticle zirconium oxide was ground to 100 mesh to obtain an inorganic powder material. According to weight parts, 50 parts of distilled water, 15 parts of NaCl, 5 parts of inorganic powder material, 2 parts of the antibacterial dispersant prepared in Example 1, 5 parts of octadecyldimethyl[3-(trimethylsilyl)propyl]ammonium chloride and 0.15 parts of antioxidant were mixed evenly to obtain an aqueous phase system; 0.1 mol / L hydrochloric acid solution was used to adjust the pH value of the aqueous phase system to 3 to obtain an aqueous phase.
[0057] A3. Preparation of composite microcapsules
[0058] According to parts by weight, 1 part of water phase and 1 part of oil phase are added to a high-speed shear emulsifier in sequence, and pre-dispersed at 1000r / min for 5-10min to obtain a pre-dispersed system; the pre-dispersed system is then transferred to a 5L reactor, and all the air in the reactor is replaced by nitrogen; the reactor is heated to 60°C for polymerization for 6h, and then the reaction is stopped, the temperature is lowered, and the material is discharged to obtain a product; the product is filtered, centrifuged and separated to obtain a solid; the solid is washed with deionized water, and then vacuum dried at 70°C to constant weight to obtain a composite microcapsule.
[0059] Example 5
[0060] This embodiment provides a method for preparing a composite microcapsule for a hygroscopic and antibacterial functional composite textile fiber, comprising the following steps:
[0061] A1. According to parts by weight, 36 parts of vinylidene fluoride, 36 parts of acrylic acid, 12 parts of methyl methacrylate, 2 parts of a crosslinking agent, 200 parts of acetone and 0.6 parts of an initiator are mixed uniformly to obtain an oil phase.
[0062] A2, inorganic nanoparticle zinc oxide was ground to 200 mesh to obtain an inorganic powder material. According to weight parts, 60 parts of distilled water, 20 parts of NaCl, 6 parts of inorganic powder material, 3 parts of antibacterial dispersant prepared in Example 2, 8 parts of octadecyldimethyl[3-(trimethylsilyl)propyl]ammonium chloride and 0.2 parts of antioxidant were mixed evenly to obtain an aqueous phase system; 0.1 mol / L hydrochloric acid solution was used to adjust the pH value of the aqueous phase system to 4 to obtain an aqueous phase.
[0063] A3. The aqueous phase and the oil phase are sequentially added to a high-speed shear emulsifier, and pre-dispersed at 11000r / min for 8min to obtain a pre-dispersed system; the pre-dispersed system is then transferred to a 5L reactor, and all the air in the reactor is replaced by nitrogen; the reactor is heated to 66°C for polymerization for 7h, and then the reaction is stopped, the temperature is lowered, and the material is discharged to obtain a product; the product is filtered, centrifuged and separated to obtain a solid; the solid is washed with deionized water, and then vacuum dried at 72°C to constant weight to obtain a composite microcapsule.
[0064] Example 6
[0065] This embodiment provides a method for preparing a composite microcapsule for a hygroscopic and antibacterial functional composite textile fiber, comprising the following steps:
[0066] A1. Evenly mix 40 parts of vinylidene fluoride, 40 parts of acrylic acid, 15 parts of methyl methacrylate, 3 g of a crosslinking agent, 200 parts of acetone and 1 part of an initiator to obtain an oil phase.
[0067] A2, inorganic nanoparticle titanium dioxide was ground to 300 mesh to obtain an inorganic powder material. According to weight parts, 80 parts of distilled water, 25 parts of NaCl, 10 parts of inorganic powder material, 5 parts of antibacterial dispersant prepared in Example 3, and 10 parts of octadecyldimethyl[3-(trimethylsilyl)propyl]ammonium chloride were mixed uniformly to obtain an aqueous phase system; 0.1 mol / L hydrochloric acid solution was used to adjust the pH value of the aqueous phase system to 4 to obtain an aqueous phase.
[0068] A3. The aqueous phase and the oil phase are sequentially added to a high-speed shear emulsifier, and pre-dispersed at 12000r / min for 10min to obtain a pre-dispersed system; the pre-dispersed system is then transferred to a 5L reactor, and all the air in the reactor is replaced by nitrogen; the reactor is then heated to 70°C for polymerization reaction for 8h, and then the reaction is stopped, the temperature is lowered, and the material is discharged to obtain a product; the product is filtered, and the sedimentation centrifugation is separated to obtain a solid; the solid is washed with deionized water, and then vacuum dried at 80°C to constant weight to obtain a composite microcapsule.
[0069] Example 7
[0070] This embodiment provides a method for preparing a hygroscopic and antibacterial functional composite textile fiber, comprising the following steps:
[0071] S1. Pure cotton yarn was soaked in 10 g / L NaOH solution with a solid-liquid ratio of 10:1, a soaking temperature of 100°C, and a soaking time of 100 min. The solution was then filtered and dried at 40°C to constant weight to obtain pretreated pure cotton yarn.
[0072] S2. Add 5 g of the composite microcapsules prepared in Example 4 into 200 mL of deionized water and mix well to obtain a functional textile liquid.
[0073] S3. Weigh the pretreated pure cotton yarn with an accuracy of 0.01g; add the pure cotton yarn to the functional textile liquid according to a bath ratio of 1:40, and heat it in a water bath to obtain the modified yarn; wherein the water bath heating temperature is 30°C and the water bath heating time is 30min, and then filter out to obtain the modified yarn; wash the modified yarn with deionized water 3 times to remove residual impurities on the surface, and then dry it in a constant temperature blast oven at 45°C to constant weight to obtain a hygroscopic and antibacterial functional fiber.
[0074] Example 8
[0075] This embodiment provides a method for preparing a hygroscopic and antibacterial functional composite textile fiber, comprising the following steps:
[0076] S1. Pure cotton yarn was soaked in 10 g / L NaOH solution with a solid-liquid ratio of 10:1, a soaking temperature of 100°C, and a soaking time of 110 min. The solution was then filtered and dried at 45°C to constant weight to obtain pretreated pure cotton yarn.
[0077] S2. Add 6 g of the composite microcapsules prepared in Example 5 into 250 mL of deionized water and mix well to obtain a functional textile liquid.
[0078] S3. Weigh the pretreated pure cotton yarn with an accuracy of 0.01g; add the pure cotton yarn to the functional textile liquid according to a bath ratio of 1:42, and heat it in a water bath to obtain the modified yarn; wherein the water bath heating temperature is 35°C, the water bath heating time is 30min, and then filter out to obtain the modified yarn; wash the modified yarn with deionized water 3 times to remove residual impurities on the surface, and then dry it in a constant temperature blast oven at 47°C to constant weight to obtain a hygroscopic and antibacterial functional fiber.
[0079] Example 9
[0080] This embodiment provides a method for preparing a hygroscopic and antibacterial functional composite textile fiber, comprising the following steps:
[0081] S1. Pure cotton yarn was soaked in 10 g / L NaOH solution with a solid-liquid ratio of 10:1, a soaking temperature of 100°C, and a soaking time of 120 min. The solution was then filtered and dried at 50°C to constant weight to obtain pretreated pure cotton yarn.
[0082] S2. Add 10 g of the composite microcapsules prepared in Example 6 into 300 mL of deionized water and mix well to obtain a functional textile liquid.
[0083] S3. Weigh the pretreated pure cotton yarn with an accuracy of 0.01g; add the pure cotton yarn to the functional textile liquid according to a bath ratio of 1:50, and heat it in a water bath, wherein the water bath heating temperature is 40°C and the water bath heating time is 30min, and then filter out to obtain the modified yarn; wash the modified yarn with deionized water 4 times to remove residual impurities on the surface, and then dry it in a constant temperature blast oven at 50°C to constant weight to obtain a hygroscopic and antibacterial functional fiber.
[0084] Comparative Example 1
[0085] The difference between this comparative example and Example 9 is that, compared with Example 6, when preparing the composite microcapsules, no antibacterial dispersant was added to the aqueous phase.
[0086] Comparative Example 2
[0087] The difference between this comparative example and Example 9 is that, compared with Example 6, when preparing the composite microcapsules, no octadecyldimethyl[3-(trimethylsilyl)propyl]ammonium chloride was added.
[0088] Comparative Example 3
[0089] The difference between this comparative example and Example 9 is that hydroxyethyl methacrylate was not added when preparing the polycondensation product.
[0090] Performance Test:
[0091] The moisture-absorbing and antibacterial functional composite textile fibers prepared in Examples 7-9 were woven with a warp density of 110 strands / inch and a weft density of 90 strands / inch to prepare textile fabrics; the above textile fabrics were labeled as Examples 10-12 in sequence.
[0092] 1. According to GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method", the antibacterial properties of the fabrics prepared in Examples 10-12 were tested, and the bacterial species used were Gram-negative bacteria Escherichia coli and Gram-positive bacteria Staphylococcus aureus.
[0093] 2. Spread the textile fabrics prepared in Examples 10-12 on the sample rack, keep the textile fabrics flat, and leave the test part suspended; drip 40 μL of 0.5% potassium dichromate solution at a time 10 cm above the textile fabrics, and measure the maximum diffusion length a and the maximum longitudinal diffusion width b of the droplets on the textile fabrics after 3 minutes. Repeat the test 5 times, and measure the mass per unit area of the textile fabrics according to GB / T4669 to obtain the water absorption rate of the textile fabrics prepared in Examples 10-12.
[0094] Moisture conduction volume: V = SH; where S is the moisture conduction area and H is the fabric thickness. The moisture conduction area is calculated using the ellipse area formula. The specific test results are shown in Table 1:
[0095] Table 1- Sample performance test data table
[0096]
[0097] Data Analysis:
[0098] A comparative analysis of the data in Table 1 above shows that the textile fabrics (Examples 10-12) prepared from the hygroscopic and antibacterial functional composite textile fibers of Examples 7-9 of the present invention all have excellent antibacterial properties, as shown by high inhibition rates against Escherichia coli and Staphylococcus aureus; however, in Comparative Example 1, no antibacterial dispersant was added when preparing the composite microcapsules; in Comparative Example 2, no octadecyldimethyl[3-(trimethylsilyl)propyl]ammonium chloride was added when preparing the composite microcapsules, thereby reducing the antibacterial properties of the prepared hygroscopic and antibacterial functional composite textile fibers and textile fabrics to varying degrees, as shown by low inhibition rates against Escherichia coli and Staphylococcus aureus.
[0099] In Comparative Example 3, hydroxyethyl methacrylate was not added when preparing the polycondensation product; the hydrophilic monomer hydroxyethyl methacrylate was removed, thereby reducing the water absorption rate of the hygroscopic and antibacterial functional composite textile fiber, thereby reducing its own hygroscopic function.
[0100] The above contents are merely examples and explanations of the structure of the present invention. The technicians in this technical field 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 structure of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.
[0101] 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.
[0102] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only specific implementation methods. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.
Claims
1. A method for preparing a hygroscopic and antibacterial functional composite textile fiber, characterized in that: The following steps are involved: S1. Soaking pure cotton yarn in NaOH solution, filtering and drying to constant weight to obtain pretreated pure cotton yarn; mixing composite microcapsules and deionized water evenly to obtain functional textile solution; S2. The pretreated pure cotton yarn and the functional textile liquid are mixed according to a bath ratio of 1:40-50, heated in a water bath, and then filtered out to obtain the modified yarn; the modified yarn is post-processed to obtain a hygroscopic and antibacterial functional fiber.
2. The method for preparing a hygroscopic and antibacterial functional composite textile fiber according to claim 1, characterized in that: The preparation method of the composite microcapsule comprises the following steps: A1, vinylidene fluoride, acrylic acid, methyl methacrylate, acetone, a crosslinking agent and an initiator are uniformly mixed to obtain an oil phase; A2, grinding inorganic nanoparticles of zirconium oxide, zinc oxide or titanium dioxide to 100-300 mesh to obtain an inorganic powder material; mixing distilled water, NaCl, inorganic powder material, antibacterial dispersant, octadecyldimethyl[3-(trimethylsilyl)propyl]ammonium chloride and antioxidant to obtain an aqueous phase system; adjusting the pH value of the aqueous phase system to 3-4 with 0.1 mol / L hydrochloric acid solution to obtain an aqueous phase; A3. The water phase and the oil phase are added to a high-speed shear emulsifier and pre-dispersed at 1000-2000 r / min for 5-10 minutes to obtain a pre-dispersed system; the pre-dispersed system is polymerized at 60-70° C. for 6-8 hours, and after post-processing, composite microcapsules are obtained.
3. The method for preparing a hygroscopic and antibacterial functional composite textile fiber according to claim 2, characterized in that: In step A1, the ratio of ethylenediaminetetrafluoroethylene, methyl methacrylate, acetone, crosslinking agent and initiator is 30-40:30-40:10-15:1-3:200:0.5-1 in parts by weight; in step A2, the ratio of distilled water, NaCl, inorganic powder material, antibacterial dispersant, octadecyldimethyl[3-(trimethylsilyl)propyl]ammonium chloride and antioxidant is 50-80:15-25:5-10:2-5:5-10:0.15-2 in parts by weight.
4. The method for preparing a hygroscopic and antibacterial functional composite textile fiber according to claim 2, characterized in that: In step A3, the ratio of the amount of the water phase to the oil phase is 1:1 in parts by weight; the post-process treatment includes: naturally cooling to room temperature to obtain a product; filtering the product, centrifuging and separating the sedimentation to obtain a solid; washing the solid with deionized water, and then vacuum drying at 70-80° C. to constant weight to obtain a composite microcapsule.
5. The method for preparing a hygroscopic and antibacterial functional composite textile fiber according to claim 1, characterized in that: The preparation method of the antibacterial dispersant comprises the following steps: B1, adipic acid, diethanolamine, hydroxyethyl methacrylate and p-toluenesulfonic acid are uniformly mixed to obtain a mixed solid-liquid; B2. The mixed solid and liquid are subjected to polycondensation reaction at 140-160° C. for 2-4 hours to obtain a product; the acidity value of the product is measured; when the conversion rate of the polycondensation reaction reaches more than 80%, the reaction is stopped and the reaction is deemed to be completed, thereby obtaining a polycondensation product; B3. Mix the polycondensation product, 2-butene-1,4-diol bis(bromoacetate), initiator BPO and ethanol, and react at 80-90° C. for 2-3 hours under a nitrogen atmosphere to obtain a product; distill the product under reduced pressure at 70-80° C. to remove the ethanol solvent to obtain a solid product; grind the solid product to 200-300 mesh to obtain an antibacterial dispersant.
6. The method for preparing a hygroscopic and antibacterial functional composite textile fiber according to claim 5, characterized in that: In step B1, the amount ratio of adipic acid, diethanolamine, hydroxyethyl methacrylate and toluenesulfonic acid is 15-30g:7-15g:13-18g:0.1-0.3g; in step B3, the amount ratio of the polycondensation product, 2-butene-1,4-diol bis(bromoacetate), initiator BPO and ethanol is 20-30g:30-40mL:0.5-1g:200mL.
7. The method for preparing a hygroscopic and antibacterial functional composite textile fiber according to claim 1, characterized in that: In step S1, the concentration of the NaOH solution is 10 g / L, and the solid-liquid ratio of the pure cotton yarn and the NaOH solution is 10:1; the soaking temperature is 10°C and the soaking time is 100-120 min; the dosage ratio of the composite microcapsule and deionized water is 5-10 g:200-300 mL; in step S2, the water bath heating temperature is 30-40°C and the water bath heating time is 30 min.
8. A hygroscopic and antibacterial functional composite textile fiber, characterized in that: The hygroscopic and antibacterial functional composite textile fiber is prepared by the preparation method of the hygroscopic and antibacterial functional composite textile fiber as described in any one of claims 1 to 7.
Citation Information
Patent Citations
Plant antibacterial and skin beautifying health-care home textile fabric and preparation method thereof
CN104178880A