Wear-resistant and antibacterial super-soft yarn and preparation method thereof

Abstract

The invention discloses a preparation method of a wear-resistant and antibacterial super soft yarn, wherein cotton fiber is sequentially subjected to pretreatment, cotton cleaning, carding, drawing, and air-spinning processes to obtain a wear-resistant and antibacterial super soft yarn; wherein the pretreatment is to impregnate the cotton fiber in an antibacterial mother liquor, and then to wash, de-dry, and dry the cotton fiber; the antibacterial mother liquor includes the following components in mass percentage: polyethylene glycol 0.6-0.8%, ethanol 12-16%, sodium chloride 0.5-1.0%, quaternary ammonium surfactant 0.5-1.5%, and the balance is water; the quaternary ammonium surfactant synergizes with polyethylene glycol and sodium chloride to significantly increase the wear-resistant, flame-retardant, and bactericidal properties of the cotton fiber. The super soft yarn provided by the present invention has excellent wear-resistant, antibacterial, and flame-retardant properties.

Description

Technical Field

[0001] The invention belongs to the technical field of textiles, and particularly relates to a wear-resistant and antibacterial super-soft yarn and a preparation method thereof. Background Art

[0002] Supersoft yarn is produced using modified special spinning equipment and a unique spinning process, resulting in a twist 20-30% lower than normal. This yarn exhibits low hairiness, high strength, low strength CV%, minimal twist unevenness, smoothness, uniform yarn length, a fluffy body, and a soft hand. It achieves a soft and comfortable feel without the need for subsequent treatment with silicone oil or softeners, making it both environmentally friendly and energy-efficient. Fabrics woven with supersoft yarn combine the soft and comfortable hand of supersoft cotton stretch fabrics with high elasticity, shaping properties, moisture wicking, and breathable, dry properties. They are widely used in sportswear, underwear, pajamas, and baby products.

[0003] The patent application number CN202010581691.4 provides a pure cotton imitation untwisted yarn super soft gauze and its preparation method, including the following steps: spinning cotton-bundle yarn-sizing-weaving-loose water washing-dehydration and drying-dyeing or printing-air beating-setting-preshrinkage-finished product. The invention uses cotton-bundle yarn to weave the cloth, and achieves fluffiness through air beating. There is no need to use water-soluble fibers to increase the strength of the yarn, ensure weaving efficiency, reduce pollutant emissions, and use physical methods to soften the fabric, which is efficient and environmentally friendly. The pure cotton imitation The untwisted super-soft gauze has a soft and fluffy feel, which effectively improves the problems of pilling and hair loss. However, people have increasingly higher requirements for the functionality of fabrics, especially the antibacterial, health-care, and wear-resistant properties of clothing. Fabrics that are in close contact with human skin will continue to be contaminated by dust, floating soil, and food stains from the human body, the outside world, and the atmospheric environment, as well as secretions such as sweat, fat, and epidermal debris from the human body. These stains can cause harmful bacteria to multiply rapidly, and the antibacterial properties of the super-soft gauze provided by this invention are difficult to meet market demand. Patent application number CN201610417459.0 provides a flame-retardant and antibacterial blended fabric comprising the following raw materials: vermiculite-modified polyester fiber, cotton fiber, modal fiber, nylon fiber, bamboo fiber, mica fiber, and Tencel. The blended fabric provided by this invention is soft, cool, pilling-resistant, breathable, and has good moisture absorption properties. It also has excellent flame retardancy and antibacterial properties. However, blended fabrics generally use a wide variety of raw materials and are complex to prepare. Furthermore, during the melt spinning process of the vermiculite and polyester masterbatch blend, the inorganic mineral vermiculite and the polyester masterbatch have poor compatibility, which in turn affects the performance of the blended fabric. Furthermore, the antibacterial effect of the blended fabric needs to be improved. Therefore, there is an urgent need to develop a wear-resistant, antibacterial, and flame-retardant pure cotton super-soft yarn. Summary of the Invention

[0004] In view of the deficiencies of the prior art, the purpose of the present invention is to provide a wear-resistant and antibacterial super-soft yarn, which has excellent wear-resistant, antibacterial, flame-retardant and other properties. The present invention also provides a preparation method of the wear-resistant and antibacterial super-soft yarn.

[0005] The technical solutions adopted by the present invention to achieve the above-mentioned purpose are:

[0006] A method for preparing a wear-resistant and antibacterial super-soft yarn comprises subjecting cotton fibers to sequential pretreatment, cleaning, carding, drawing, and air-spinning processes to produce the wear-resistant and antibacterial super-soft yarn; wherein the pretreatment comprises immersing the cotton fibers in an antibacterial mother liquor, followed by washing, desiccation, and drying; the antibacterial mother liquor comprises the following components in percentage by weight: 0.6-0.8% polyethylene glycol, 12-16% ethanol, 0.5-1.0% sodium chloride, 0.5-1.5% quaternary ammonium surfactant, and the balance being water; and the preparation method of the quaternary ammonium surfactant is as follows:

[0007] S1. While stirring, heat propyl ethylene oxide to 60-70°C, add dibutyl phosphate dropwise, complete the addition over 0.5-1.5 hours, then heat to 85-95°C, continue stirring for 3-5 hours, and cool to room temperature to obtain intermediate 1;

[0008] S2. Disperse 4-dimethylaminobutyric acid in N,N-dimethylformamide, add p-toluenesulfonic acid and the intermediate 1 obtained in step S1 in sequence, heat to 55-70° C., react for 4-9 hours, cool to room temperature, then add deionized water and sodium bicarbonate in sequence, stir for 20-30 minutes, extract, and distill under reduced pressure to obtain intermediate 2;

[0009] S3. Under a nitrogen atmosphere, the intermediate 2 obtained in step S2 and 1-chlorobutane are dispersed in acetonitrile, potassium iodide is added, the temperature is raised to 75-90°C, and the reaction is stirred for 12-18 hours. The mixture is subjected to reduced pressure distillation, extraction, back extraction, and concentration and drying to obtain a quaternary ammonium surfactant;

[0010] The synthetic route of quaternary ammonium surfactants is as follows:

[0011]

[0012]

[0013] The present invention uses propyl ethylene oxide and dibutyl phosphate as raw materials, and undergoes a ring-opening reaction of the epoxy compound under heating conditions to obtain an intermediate 1; the intermediate 1 undergoes an esterification reaction with 4-dimethylaminobutyric acid under the action of p-toluenesulfonic acid to obtain an intermediate 2; and the tertiary amine in the structure of the intermediate 2 further undergoes a quaternization reaction with 1-chlorobutane to obtain a quaternary ammonium salt surfactant.

[0014] In order to obtain a quaternary ammonium surfactant and ensure product consistency, the molar ratio of propyl ethylene oxide to dibutyl phosphate in step S1 is 1:0.9-1.2; the molar ratio of 4-dimethylaminobutyric acid, p-toluenesulfonic acid and intermediate 1 in step S2 is 1:0.04-0.08:0.8-1.0, the amount of 4-dimethylaminobutyric acid added to N,N-dimethylformamide is 0.15-0.40 g / mL, and the mass ratio of p-toluenesulfonic acid, deionized water and sodium bicarbonate is 3-6:25-45:2-5; the molar ratio of intermediate 2, 1-chlorobutane and potassium iodide in step S3 is 1:0.9-1.4:0.2-0.5, and the amount of intermediate 2 added to acetonitrile is 0.3-0.7 g / mL.

[0015] Preferably, the immersion temperature is 30-45° C. and the immersion time is 2-4 hours.

[0016] The antibacterial mother solution comprises the following raw materials: polyethylene glycol, ethanol, sodium chloride, and a quaternary ammonium surfactant. Both polyethylene glycol and sodium chloride have bactericidal and antiseptic effects. Quaternary ammonium salt-type cationic active bactericides are safe for human health and are widely used for bactericidal, disinfectant, and antiseptic use in the fields of medicine and daily chemicals due to their advantages of low toxicity, high efficiency, and broad spectrum. Single-component bactericides can cause bacteria to develop resistance. The compounding of polyethylene glycol, sodium chloride, and a quaternary ammonium surfactant not only takes into account both chemical safety and economic rationality, but also significantly increases the bactericidal performance of the product. Furthermore, the good film-forming property of polyethylene glycol can significantly improve the wear resistance of the product.

[0017] The present invention has the following beneficial effects: the present invention synthesizes a quaternary ammonium surfactant through a three-step process, wherein the quaternary ammonium surfactant contains a phosphate group, a carboxylate group, and a quaternary ammonium salt structure. The phosphate group and the carboxylate group act synergistically to significantly improve the flame retardant properties of the quaternary ammonium surfactant; the quaternary ammonium salt, polyethylene glycol, and sodium chloride synergize to achieve both chemical safety and economic rationality while significantly enhancing the bactericidal properties of the product; and the polyethylene glycol has good film-forming properties and can significantly improve the wear resistance of cotton fibers. The present invention pre-treats the cotton fibers with an antibacterial mother liquor, and then undergoes cleaning, carding, drawing, and air-spinning processes to obtain a super-soft yarn having excellent wear resistance, antibacterial, and flame retardant properties. DETAILED DESCRIPTION

[0018] The following will be combined with the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the embodiments described are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in this application, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of this application. The raw materials used in the following examples are all common commercially available products.

[0019] Example 1

[0020] A method for preparing a quaternary ammonium salt surfactant comprises the following steps:

[0021] S1. Under stirring conditions, propyl oxirane was heated to 65°C, and dibutyl phosphate was added dropwise. The addition was completed over 1 hour, and the temperature was then raised to 85°C. Stirring was continued for 4 hours, and the mixture was cooled to room temperature to obtain intermediate 1, wherein the molar ratio of propyl oxirane to dibutyl phosphate was 1:1.1;

[0022] S2. Disperse 4-dimethylaminobutyric acid in N,N-dimethylformamide, add p-toluenesulfonic acid and the intermediate 1 obtained in step S1 in sequence, heat to 60°C, react for 5h, cool to room temperature, and then add deionized water and sodium bicarbonate in sequence, stir for 30min, extract with ethyl acetate, and distill the organic phase under reduced pressure to obtain intermediate 2, wherein the molar ratio of 4-dimethylaminobutyric acid, p-toluenesulfonic acid and intermediate 1 is 1:0.05:0.9, the amount of 4-dimethylaminobutyric acid added to N,N-dimethylformamide is 0.3g / mL, and the mass ratio of p-toluenesulfonic acid, deionized water and sodium bicarbonate is 5:40:4;

[0023] S3, under a nitrogen atmosphere, the intermediate obtained in step S2 and 1-chlorobutane are dispersed in acetonitrile, potassium iodide is added, the temperature is raised to 80 ° C, and the stirring reaction is 16h. Acetonitrile is removed by distillation under reduced pressure, and deionized water and ethyl acetate are added for extraction. The organic phase is reversed and extracted once, and the resulting aqueous phase is combined and concentrated and dried to obtain a quaternary ammonium surfactant, wherein the molar ratio of intermediate 2, 1-chlorobutane and potassium iodide is 1:1.2:0.4, and the addition amount of intermediate 2 in acetonitrile is 0.6g / mL, and the volume ratio of deionized water and ethyl acetate is 1:1;

[0024] The synthetic route of quaternary ammonium surfactants is as follows:

[0025]

[0026]

[0027] The NMR results of quaternary ammonium surfactants are: 1H NMR (300MHz, D2O) δ4.55-4.59 (m, 1H), 4.35-4.38 (m, 1H), 4.12-4.15 (m, 1H), 4.04 (t, 4H), 2.33-2.37 (m, 6H), 2.27 (s, 6H), 1.87-1.8 9(m, 2H), 1.65-1.68(m, 4H), 1.47-1.51(m, 2H), 1.40-1.44(m, 4H), 1.34-1.36(m, 2H), 1.27-1.31(m, 4H), 0.95(t, 6H), 0.88(t, 6H).

[0028] Example 2

[0029] A method for preparing a wear-resistant and antibacterial super-soft yarn comprises the following steps:

[0030] (1) Pretreatment: Prepare an antibacterial mother solution (comprising the following components in percentage by mass: 0.8% polyethylene glycol, 14% ethanol, 0.6% sodium chloride, 0.9% quaternary ammonium salt surfactant prepared in Example 1, and the balance being water), immerse cotton fibers (fineness 1.56 dtex, length 38 mm) in the antibacterial mother solution at a temperature of 40° C. for 3 h, rinse in clean water at 30° C. after immersion, dehydrate in a centrifugal dehydrator, and finally dry at 70° C. to obtain treated cotton fibers;

[0031] (2) Cotton cleaning: The pretreated cotton fibers are sequentially processed using a plucker, a heavy object separator, a single-axis flow cotton opener, a ten-bin cotton blender, a fine cotton opener, and a dust reduction machine to obtain combed cotton fiber rolls. The beater speed of the plucker is 580 r / min, and the beater speed of the fine cotton opener is 500 r / min. The beaters are comb-pin type beaters.

[0032] (3) Combing: The combed cotton fiber roll is fed into the carding machine to obtain cotton fiber strips, wherein the sliver weight of the cotton fiber is 16.5g / 5m, the cylinder speed of the carding machine is 270r / min, the licker-in speed is 560r / min, the cover speed is 100mm / min, the doffer speed is 35r / min, the distance between the feed plate and the licker-in is 0.35mm, the distance between the licker-in and the cylinder is 0.16mm, and the distance between the cylinder and the front carding plate is 0. The gauges are 0.25mm, 0.21mm, and 0.17mm, the gauges between the cylinder and the doffer are 0.12mm, the gauges between the cylinder and the flat are 0.19mm, 0.16mm, 0.16mm, 0.14mm, and 0.17mm, the gauges between the cylinder and the front fixed flat are 0.80mm, 0.27mm, and 0.60mm, the gauges between the cylinder and the rear fixed flat are 0.45mm and 0.55mm, and the delivery speed is 110m / min.

[0033] (4) Drawing: The cotton fiber strips are fed into the drawing frame to obtain cotton strips, wherein the drawing speed of the drawing frame is 160m / min, the basis weight of the drawing frame is 20.2g / 5m, 6 strands are combined, the back drafting zone is 1.5 times, and the roller gauge is 14mm*20mm; the basis weight of the second pass is 18.0g / 5m, 6 strands are combined, the total draft is 6.16 times, the back zone draft is 1.3 times, and the roller gauge is 6mm*15mm;

[0034] (5) Air-spinning: The cotton strips are fed into the air-spinning machine. After the air-spinning is completed, the super soft yarn is obtained. The air-spinning rotor speed is 25000r / min, the combing roller speed is 6100r / min, the twist is 125 twists / 10cm, and the twist coefficient is 450.

[0035] Example 3

[0036] A method for preparing a wear-resistant and antibacterial ultra-soft yarn is prepared according to the method of Example 2, except that the mass percentage of the quaternary ammonium salt surfactant is changed to 0.5%.

[0037] Example 4

[0038] A method for preparing a wear-resistant and antibacterial ultra-soft yarn is prepared according to the method of Example 2, except that the mass percentage of the quaternary ammonium salt surfactant is changed to 1.5%.

[0039] Comparative Example 1

[0040] A method for preparing wear-resistant and antibacterial ultra-soft yarn is prepared according to the method of Example 2, except that the quaternary ammonium salt surfactant is replaced by hexadecyltrimethylammonium bromide.

[0041] Comparative Example 2

[0042] A method for preparing a wear-resistant and antibacterial ultra-soft yarn is prepared according to the method of Example 2, except that no quaternary ammonium surfactant is added.

[0043] Relevant performance tests were performed on the wear-resistant and antibacterial super-soft yarns prepared in Examples 2-4 and Comparative Examples 1-2. The abrasion resistance test was carried out in accordance with the standard ASTM D 3108-2001 test method for the coefficient of friction between yarn and solid material; the samples prepared in Examples 2-4 and Comparative Examples 1-2 were woven into fabrics and then subjected to antibacterial performance testing. The test was carried out in accordance with GB / T20944.3-2008 "Evaluation of Antibacterial Properties of Textiles Part 3: Oscillation Method", using a washing color fastness tester washing method, and the antibacterial rate of the fabric after washing 30 times was tested; the samples prepared in Examples 2-4 and Comparative Examples 1-2 were woven into fabrics and then subjected to flame retardant performance testing in accordance with the national standard GB / T17591-2006 for flame retardant fabrics. Grade B1: damaged length ≤150 mm, afterflaming time ≤5 s, smoldering time ≤5 s; Grade B2: damaged length ≤200 mm, afterflaming time ≤15 s, smoldering time ≤15 s; the results are shown in Table 1. As can be seen from the table, the antibacterial performance, wear resistance and flame retardant performance of the super soft yarn prepared in Examples 2-4 are significantly better than those in Comparative Examples 1-2. The antibacterial rate of the super soft yarn prepared in Examples 2 and 4 is still 100% after being washed 30 times. Compared with Comparative Example 2, the quaternary ammonium salt surfactant added in Example 2 can significantly improve the antibacterial performance, wear resistance and flame retardant performance of the super soft yarn.

[0044] Table 1 Super soft yarn performance test results

[0045]

[0046] The invention synthesizes a quaternary ammonium surfactant by a three-step method. The quaternary ammonium surfactant contains a phosphate group, a carboxylate group and a quaternary ammonium salt structure. An antibacterial mother liquor containing polyethylene glycol, ethanol, sodium chloride and the quaternary ammonium surfactant is prepared. Cotton fibers are pretreated with the antibacterial mother liquor. The super-soft yarn obtained by the cotton cleaning, carding, drawing and air-spinning processes has excellent wear resistance, antibacterial and flame retardant properties.

[0047] Although the embodiments of the present application have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and variations may be made to these embodiments without departing from the principles and spirit of the present application, and the scope of the present application is defined by the appended claims and their equivalents.

Claims

1. A method for preparing wear-resistant and antibacterial super-soft yarn, characterized in that: Cotton fibers are sequentially subjected to pretreatment, cleaning, carding, drawing, and air-spinning processes to produce wear-resistant and antibacterial ultra-soft yarn; wherein the pretreatment comprises immersing the cotton fibers in an antibacterial mother liquor, followed by washing, drying, and drying; the antibacterial mother liquor comprises the following components in percentage by weight: 0.6-0.8% polyethylene glycol, 12-16% ethanol, 0.5-1.0% sodium chloride, 0.5-1.5% quaternary ammonium surfactant, and the balance water; The preparation method of described quaternary ammonium salt surfactant is as follows: S1. Under stirring conditions, propyl ethylene oxide was heated to 60-70°C, and dibutyl phosphate was added dropwise. The addition was completed over 0.5-1.5 hours. The temperature was then raised to 85-95°C, and stirring was continued for 3-5 hours. The mixture was cooled to room temperature to obtain intermediate 1. The structural formula of intermediate 1 is: S2. Disperse 4-dimethylaminobutyric acid in N,N-dimethylformamide, add p-toluenesulfonic acid and the intermediate 1 obtained in step S1 in sequence, heat to 55-70°C, react for 4-9 hours, cool to room temperature, then add deionized water and sodium bicarbonate in sequence, stir for 20-30 minutes, extract, and distill under reduced pressure to obtain intermediate 2. The structural formula of intermediate 2 is: S3. Under a nitrogen atmosphere, the intermediate 2 obtained in step S2 and 1-chlorobutane are dispersed in acetonitrile, potassium iodide is added, the temperature is raised to 75-90° C., and the reaction is stirred for 12-18 hours. The mixture is subjected to reduced pressure distillation, extraction, back extraction, and concentration and drying to obtain a quaternary ammonium surfactant. The structural formula of the quaternary ammonium surfactant is:

2. The wear-resistant and antibacterial super soft yarn prepared by the method according to claim 1.

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