High-elasticity anti-static modified nylon fabric and preparation method thereof

Abstract

The present application relates to a kind of high elastic anti-static modified nylon fabric and its preparation method, belong to textile technical field.The present application provides a kind of preparation method of high elastic anti-static modified nylon fabric, summarized as nonionic surface active solution treatment is carried out to nylon fabric, then immersed in benzyl alcohol solution, then mixed with polyether amine solution to realize modification, finally after covering, finishing after conductive slurry is obtained.The present application improves elasticity by swelling-grafting, then carries out conductive covering, avoids the formation of elastic network by conductive material interference, the flexible segment of polyether amine and the rigidity of conductive carbon material are complementary, improve elastic recovery rate, in the case where high elasticity is maintained, not to destroy conductive path after being stretched for many times, play anti-static effect, to effectively improve the elasticity and antistatic property of nylon fabric overall, improve the experience of wearing nylon fabric product.

Description

Technical Field

[0001] This invention belongs to the field of textile technology and relates to a highly elastic and antistatic modified nylon fabric and its preparation method. Background Technology

[0002] As people's living standards improve and their attitudes change, consumers are paying more and more attention to the quality of clothing. Compared to other materials, nylon has good abrasion resistance and elasticity, and is often used to make underwear and nylon fabrics. It is suitable for everyday wear, fitting well without feeling restrictive, and is not easily damaged after washing, possessing a certain degree of durability. However, nylon has poor moisture absorption, which means that the surface charge of the fabric cannot be discharged in time, and static electricity is easily accumulated. In addition, when nylon fabric is worn close to the skin, it is easy to generate static electricity through friction with the skin and outer clothing, exacerbating static electricity accumulation and thus affecting the wearing experience. Summary of the Invention

[0003] The purpose of this invention is to provide a highly elastic and antistatic modified nylon fabric and its preparation method. This invention improves elasticity through swelling and grafting, and then applies conductive coating to avoid the conductive material interfering with the formation of the elastic network. The flexible segments of polyetheramine and the rigidity of conductive carbon material complement each other, so that the conductive path is not destroyed after multiple stretching while maintaining high elasticity, thus achieving the antistatic effect.

[0004] The objective of this invention can be achieved through the following technical solutions:

[0005] A method for preparing a highly elastic, antistatic modified nylon fabric, the method comprising the following steps:

[0006] Step 1: Immerse the nylon fabric in a non-ionic surfactant solution, wash with water until neutral, and dehydrate to obtain the treated nylon fabric.

[0007] Step 2: Immerse the treated nylon fabric in a benzyl alcohol solution to swell, then dry it to obtain the swollen nylon fabric.

[0008] Step 3: Mix the swollen nylon fabric with the polyetheramine solution, wash with acetone to remove unreacted monomers, and dry to obtain the modified nylon fabric.

[0009] Step 4: Mix the modified nylon fabric with the conductive paste, sonicate, perform gradient drying, and plasma treatment to obtain the conductive nylon fabric.

[0010] Step 5: Perform post-treatment on the conductive nylon fabric to obtain the final product.

[0011] Further, the nonionic surfactant solution in step one is an aqueous solution containing 1-2 wt% Triton X-100; the dehydration refers to dehydration to a water content of 10-20 wt%.

[0012] Further, the benzaldehyde content in the benzaldehyde solution in step two is 35-45 wt%; the swelling refers to swelling by constant temperature oscillation at 48-52℃ for 30-40 minutes, with an oscillation frequency of 60-80 rpm; the drying refers to drying with hot air circulation at 80℃ until the moisture content is less than 3%.

[0013] Further, in step three, the mass ratio of the swollen nylon fabric to the polyetheramine solution is 1:18-20; the polyetheramine solution is obtained by mixing polyetheramine, HDI trimer, and 68-74wt% ethanol solution in a mass ratio of 1.2-1.4:2-3:8.6-9; the mixing refers to adjusting the pH to 8.3-8.5 with triethylamine, shaking at 40-44℃ for 2-3 hours, pre-drying at 80℃ for 30-40 minutes after shaking, and then heat-curing at 120℃ for 40-50 minutes; the drying temperature is 80℃.

[0014] Further, in step four, the mass ratio of the modified nylon fabric to the conductive paste is 1:12-16; the ultrasonication refers to setting the ultrasonic frequency to 40-50kHz, the ultrasonic power to 100-200W, the ultrasonic temperature to 45-55℃, and the ultrasonic treatment time to 30-40min; the gradient drying refers to drying at 60℃ for 20-26min first, and then drying at 100℃ for 14-16min; the plasma treatment refers to setting the power to 200-300W, the processing speed to 2-4m / min, introducing 18-22wt% oxygen and the remainder argon, and performing plasma treatment for 3-5min.

[0015] Furthermore, the method for preparing the conductive paste in step four includes the following steps:

[0016] Step Z1: Polyvinylpyrrolidone and deionized water are stirred at 40-50℃ for 25-35 min to prepare a polyvinylpyrrolidone solution with a total polyvinylpyrrolidone content of 1-2 wt%.

[0017] Step Z2: Add graphene-coated carbon nanotube powder to a polyvinylpyrrolidone solution, stir at 500-700 rpm for 20-30 min, then shear and disperse, cool, and obtain a slurry;

[0018] Step Z3: Add 5-6 wt% of waterborne polyurethane to the slurry at a dropping rate of 0.5-1.5 mL / min, stir at 400-600 rpm until the dropping is finished, homogenize under high pressure at 800-1200 bar three times, each time for 1-3 min, then stir at 250-350 rpm for 0.8-1.2 h, let stand at room temperature for 24-28 h, and filter through a 200-mesh screen to obtain the final product.

[0019] Further, in step Z2, the total amount of graphene-coated carbon nanotube powder is 14-16 wt% of the slurry; the shear dispersion refers to stirring at 2500-3500 rpm for 8-12 min, then stirring at 7000-9000 rpm for 25-35 min, and finally setting the ultrasonic frequency to 40-50 kHz, the ultrasonic power to 250-350 W, and sonicating for 18-22 min.

[0020] Furthermore, the preparation method of the graphene-coated carbon nanotube powder in step Z2 includes the following steps:

[0021] Step Y1: Mix graphene oxide, carboxylated carbon nanotubes, and deionized water in a mass ratio of 1:2.8-3.2:90-110, set the ultrasonic frequency to 30-50kHz, the ultrasonic power to 300-400W, and sonicate for 20-40 minutes to obtain a suspension.

[0022] Step Y2: Mix KH-550 and the suspension at a mass ratio of 1:66.5-67.1, and stir in an oil bath at 80℃ and a speed of 800-1000rpm for 3-4 hours to obtain the reaction solution;

[0023] Step Y3: Centrifuge the reaction solution to collect the precipitate, wash it three times with anhydrous ethanol, and dry it under vacuum at 60℃ for 24-32 hours to obtain the final product.

[0024] Further, the finishing process described in step five refers to immersing the conductive-treated nylon fabric in an aqueous solution of amino silicone oil containing 5-7 wt% amino silicone oil until the roll yield is 78-82%, baking at 105-115℃ for 2-4 minutes, and then heat-setting at 158-162℃ for 25-35 seconds.

[0025] Furthermore, the modified nylon fabric is used to prepare underwear and nylon fabric.

[0026] The beneficial effects of this invention are:

[0027] (1) Before the modification treatment, the fiber is swollen with benzyl alcohol solution to expand the free volume inside the fiber. On this basis, flexible segments are introduced. The polyetheramine molecular backbone contains ether bonds. The rotatability of the ether bonds through the interaction between HDI trimer and nylon terminal amino groups gives the network dynamic properties. When subjected to force, it can dissipate energy and improve the elastic recovery rate.

[0028] (2) In this invention, both graphene oxide and carbon nanotubes are carbon-based conductive materials. The two-dimensional sheet structure of graphene can wrap the surface of carbon nanotubes to form a three-dimensional conductive network, thereby achieving an antistatic effect by reducing the volume resistivity of the fiber. On this basis, KH-550 is introduced to form a chemical bond between the carbon material and the matrix interface, thereby improving the interfacial bonding strength. Plasma treatment is used to increase the specific surface area and introduce oxygen-containing groups, which further enhances the bonding between the conductive layer and the matrix and avoids delamination.

[0029] (3) This invention improves elasticity through swelling-grafting and then applies conductive coating to avoid the conductive material interfering with the formation of the elastic network. The flexible segments of polyetheramine and the rigidity of conductive carbon material complement each other. While maintaining high elasticity, the conductive path is not destroyed after multiple stretching, thus playing an antistatic effect. This effectively improves the overall elasticity and antistatic properties of nylon fabric and enhances the wearing experience of nylon fabric products. Detailed Implementation

[0030] To further illustrate the technical means and effects of the present invention in achieving its intended purpose, the following detailed description of the specific implementation methods, structures, features, and effects of the present invention, in conjunction with embodiments, is provided below.

[0031] In all embodiments and comparative examples of this invention, the nylon fabric used was nylon 6, which was purchased directly from the market from Shanghai Kairuixiang New Material Co., Ltd.; Triton X-100, benzaldehyde, ethanol, polyvinylpyrrolidone, and graphene oxide were all purchased directly from the market from Sigma-Aldrich (Shanghai) Trading Co., Ltd.; polyetheramine was purchased directly from the market from Hubei Xinyuhong Biomedical Technology Co., Ltd.; HDI trimer was purchased directly from the market from Hubei Langbowan Biomedical Co., Ltd.; triethylamine was purchased directly from the market from Jinan Renyuan Chemical Co., Ltd.; waterborne polyurethane was purchased directly from the market from Jining Tangyi Chemical Co., Ltd., CAS number 9009-54-5; carboxylated carbon nanotubes with a diameter of 10nm and a length of 1μm were purchased directly from the market from Guangzhou Hongwu Materials Technology Co., Ltd.; amino silicone oil was purchased directly from the market from Shandong Huling New Materials Co., Ltd., CAS number 63148-62-0; KH-550 was purchased directly from the market from Wuhan Smike Biotechnology Co., Ltd.

[0032] In all embodiments and comparative examples of this invention, the nylon fabrics have undergone conventional steps such as opening, cleaning, and mixing before processing.

[0033] Example 1

[0034] A method for preparing a highly elastic, antistatic modified nylon fabric, the method comprising the following steps:

[0035] Step 1: Immerse the nylon fabric in a non-ionic surfactant solution, wash with water until neutral, and dehydrate to obtain the treated nylon fabric.

[0036] Step 2: Immerse the treated nylon fabric in a benzyl alcohol solution to swell, then dry it to obtain the swollen nylon fabric.

[0037] Step 3: Mix the swollen nylon fabric with the polyetheramine solution, wash with acetone to remove unreacted monomers, and dry to obtain the modified nylon fabric.

[0038] Step 4: Mix the modified nylon fabric with the conductive paste, sonicate, perform gradient drying, and plasma treatment to obtain the conductive nylon fabric.

[0039] Step 5: Perform post-treatment on the conductive nylon fabric to obtain the final product.

[0040] The nonionic surfactant solution mentioned in step one is an aqueous solution containing 1 wt% Triton X-100; the dehydration refers to dehydration to a water content of 10 wt%.

[0041] The benzaldehyde content in the benzaldehyde solution in step two is 35 wt%; the swelling refers to swelling by constant temperature oscillation at 48°C for 30 min at an oscillation frequency of 60 rpm; the drying refers to drying by hot air circulation at 80°C until the moisture content is less than 3%.

[0042] The mass ratio of the swollen nylon fabric to the polyetheramine solution in step three is 1:18; the polyetheramine solution is obtained by mixing polyetheramine, HDI trimer, and 68-74wt% ethanol solution in a mass ratio of 1.2:2:8.6; the mixing refers to adjusting the pH to 8.3 with triethylamine, shaking at 40℃ for 2 hours, pre-drying at 80℃ for 30 minutes after shaking, and then heat curing at 120℃ for 40 minutes; the drying temperature is 80℃.

[0043] The mass ratio of the modified nylon fabric to the conductive paste in step four is 1:12; the ultrasonication refers to setting the ultrasonic frequency to 40kHz, the ultrasonic power to 100W, the ultrasonic temperature to 45℃, and ultrasonication for 30 minutes; the gradient drying refers to drying at 60℃ for 20 minutes first, and then drying at 100℃ for 14 minutes; the plasma treatment refers to setting the power to 200W, the processing speed to 2m / min, introducing 18wt% oxygen and the remainder argon, and plasma treatment for 3 minutes.

[0044] The preparation method of the conductive paste described in step four includes the following steps:

[0045] Step Z1: Polyvinylpyrrolidone and deionized water are stirred at 40°C for 25 min to prepare a polyvinylpyrrolidone solution with a total polyvinylpyrrolidone content of 1 wt%.

[0046] Step Z2: Add graphene-coated carbon nanotube powder to polyvinylpyrrolidone solution, stir at 500 rpm for 20 min, then shear disperse, cool, and obtain slurry;

[0047] Step Z3: Add 5 wt% of waterborne polyurethane to the slurry at a dropping rate of 0.5 mL / min, stir at 400 rpm until the dropping is finished, homogenize at 800 bar for 1 min each time, stir at 250 rpm for 0.8 h, let stand at room temperature for 24 h, and filter through a 200 mesh screen to obtain the final product.

[0048] The total amount of graphene-coated carbon nanotube powder in step Z2 is 14 wt% of the slurry; the shear dispersion refers to stirring at 2500 rpm for 8 min, then stirring at 7000 rpm for 25 min, and finally setting the ultrasonic frequency to 40 kHz, the ultrasonic power to 250 W, and sonicating for 18 min.

[0049] The preparation method of graphene-coated carbon nanotube powder in step Z2 includes the following steps:

[0050] Step Y1: Mix graphene oxide, carboxylated carbon nanotubes, and deionized water in a mass ratio of 1:2.8:90, set the ultrasonic frequency to 30kHz and the ultrasonic power to 300W, and sonicate for 20 minutes to obtain a suspension.

[0051] Step Y2: KH-550 and the suspension are mixed at a mass ratio of 1:66.51 and stirred in an oil bath at 80°C and 800 rpm for 3 hours to obtain the reaction solution.

[0052] Step Y3: Centrifuge the reaction solution to collect the precipitate, wash it three times with anhydrous ethanol, and dry it under vacuum at 60℃ for 24 hours to obtain the final product.

[0053] Step 5 refers to the finishing process of immersing the conductive nylon fabric in an amino silicone oil aqueous solution containing 5 wt% amino silicone oil until the roll-off rate is 78%, baking at 105°C for 2 minutes, and then heat-setting at 158°C for 25 seconds.

[0054] The modified nylon fabric is used to prepare underwear and nylon cloth.

[0055] Example 2

[0056] A method for preparing a highly elastic, antistatic modified nylon fabric, the method comprising the following steps:

[0057] Step 1: Immerse the nylon fabric in a non-ionic surfactant solution, wash with water until neutral, and dehydrate to obtain the treated nylon fabric.

[0058] Step 2: Immerse the treated nylon fabric in a benzyl alcohol solution to swell, then dry it to obtain the swollen nylon fabric.

[0059] Step 3: Mix the swollen nylon fabric with the polyetheramine solution, wash with acetone to remove unreacted monomers, and dry to obtain the modified nylon fabric.

[0060] Step 4: Mix the modified nylon fabric with the conductive paste, sonicate, perform gradient drying, and plasma treatment to obtain the conductive nylon fabric.

[0061] Step 5: Perform post-treatment on the conductive nylon fabric to obtain the final product.

[0062] The nonionic surfactant solution mentioned in step one is an aqueous solution containing 1.2 wt% Triton X-100; the dehydration refers to dehydration to a water content of 13 wt%.

[0063] The benzaldehyde content in the benzaldehyde solution in step two is 38 wt%; the swelling refers to swelling by constant temperature oscillation at 49°C for 32 minutes at an oscillation frequency of 65 rpm; the drying refers to drying by hot air circulation at 80°C until the moisture content is less than 3%.

[0064] The mass ratio of the swollen nylon fabric to the polyetheramine solution in step three is 1:18.6; the polyetheramine solution is obtained by mixing polyetheramine, HDI trimer, and 68-74 wt% ethanol solution in a mass ratio of 1.27:2.4:8.7; the mixing refers to adjusting the pH to 8.3 with triethylamine, shaking at 41°C for 2.1 h, pre-drying at 80°C for 33 min after shaking, and then heat curing at 120°C for 42 min; the drying temperature is 80°C.

[0065] The mass ratio of the modified nylon fabric to the conductive paste in step four is 1:13; the ultrasonication refers to setting the ultrasonic frequency to 44kHz, the ultrasonic power to 120W, the ultrasonic temperature to 48℃, and ultrasonication for 32 minutes; the gradient drying refers to drying at 60℃ for 21 minutes first, and then drying at 100℃ for 14.5 minutes; the plasma treatment refers to setting the power to 230W, the processing speed to 2.5m / min, introducing 19wt% oxygen and the remainder argon, and plasma treatment for 3.5 minutes.

[0066] The preparation method of the conductive paste described in step four includes the following steps:

[0067] Step Z1: Polyvinylpyrrolidone and deionized water were stirred at 42°C for 28 min to prepare a polyvinylpyrrolidone solution with a total polyvinylpyrrolidone content of 1.3 wt%.

[0068] Step Z2: Add graphene-coated carbon nanotube powder to polyvinylpyrrolidone solution, stir at 570 rpm for 24 min, then shear dispersion, cool to obtain slurry;

[0069] Step Z3: Add 5.2 wt% of waterborne polyurethane to the slurry at a dropping rate of 0.8 mL / min, stir at 460 rpm until the dropping is finished, homogenize at 900 bar for 1.5 min each time, stir at 280 rpm for 0.9 h, let stand at room temperature for 25 h, and filter through a 200 mesh screen to obtain the final product.

[0070] The total amount of graphene-coated carbon nanotube powder in step Z2 is 14.5 wt% of the slurry; the shear dispersion refers to stirring at 2900 rpm for 9 min, then stirring at 7400 rpm for 28 min, and finally setting the ultrasonic frequency to 42 kHz, the ultrasonic power to 260 W, and sonicating for 19 min.

[0071] The preparation method of graphene-coated carbon nanotube powder in step Z2 includes the following steps:

[0072] Step Y1: Mix graphene oxide, carboxylated carbon nanotubes, and deionized water in a mass ratio of 1:2.9:97, set the ultrasonic frequency to 35kHz and the ultrasonic power to 310W, and sonicate for 25 minutes to obtain a suspension.

[0073] Step Y2: KH-550 and the suspension are mixed at a mass ratio of 1:66.7 and stirred in an oil bath at 80℃ and 850 rpm for 3.2 hours to obtain the reaction solution;

[0074] Step Y3: Centrifuge the reaction solution to collect the precipitate, wash it three times with anhydrous ethanol, and dry it under vacuum at 60℃ for 26 hours to obtain the final product.

[0075] The finishing process described in step five refers to immersing the conductive-treated nylon fabric in an aqueous solution of amino silicone oil containing 5.8 wt% amino silicone oil until the roll-off rate is 79%, baking at 108°C for 2.6 min, and then heat-setting at 159°C for 28 s.

[0076] The modified nylon fabric is used to prepare underwear and nylon cloth.

[0077] Example 3

[0078] A method for preparing a highly elastic, antistatic modified nylon fabric, the method comprising the following steps:

[0079] Step 1: Immerse the nylon fabric in a non-ionic surfactant solution, wash with water until neutral, and dehydrate to obtain the treated nylon fabric.

[0080] Step 2: Immerse the treated nylon fabric in a benzyl alcohol solution to swell, then dry it to obtain the swollen nylon fabric.

[0081] Step 3: Mix the swollen nylon fabric with the polyetheramine solution, wash with acetone to remove unreacted monomers, and dry to obtain the modified nylon fabric.

[0082] Step 4: Mix the modified nylon fabric with the conductive paste, sonicate, perform gradient drying, and plasma treatment to obtain the conductive nylon fabric.

[0083] Step 5: Perform post-treatment on the conductive nylon fabric to obtain the final product.

[0084] The nonionic surfactant solution mentioned in step one is an aqueous solution containing 1.5 wt% Triton X-100; the dehydration refers to dehydration to a water content of 15 wt%.

[0085] The benzaldehyde content in the benzaldehyde solution in step two is 40 wt%; the swelling refers to swelling by constant temperature oscillation at 50°C for 35 minutes at an oscillation frequency of 70 rpm; the drying refers to drying by hot air circulation at 80°C until the moisture content is less than 3%.

[0086] The mass ratio of the swollen nylon fabric to the polyetheramine solution in step three is 1:19; the polyetheramine solution is obtained by mixing polyetheramine, HDI trimer, and 71wt% ethanol solution in a mass ratio of 1.3:2.5:8.8; the mixing refers to adjusting the pH to 8.4 with triethylamine, shaking at 42℃ for 2.5h, pre-drying at 80℃ for 35min after shaking, and then heat curing at 120℃ for 45min; the drying temperature is 80℃.

[0087] The mass ratio of the modified nylon fabric to the conductive paste in step four is 1:14; the ultrasonication refers to setting the ultrasonic frequency to 45kHz, the ultrasonic power to 150W, the ultrasonic temperature to 50℃, and ultrasonication for 35 minutes; the gradient drying refers to drying at 60℃ for 23 minutes first, and then drying at 100℃ for 15 minutes; the plasma treatment refers to setting the power to 250W, the processing speed to 3m / min, introducing 20wt% oxygen and the remainder argon, and plasma treatment for 4 minutes.

[0088] The preparation method of the conductive paste described in step four includes the following steps:

[0089] Step Z1: Polyvinylpyrrolidone and deionized water were stirred at 45°C for 30 min to prepare a polyvinylpyrrolidone solution with a total polyvinylpyrrolidone content of 1.5 wt%.

[0090] Step Z2: Add graphene-coated carbon nanotube powder to polyvinylpyrrolidone solution, stir at 600 rpm for 25 min, then shear disperse, cool, and obtain slurry;

[0091] Step Z3: Add 5.5 wt% of waterborne polyurethane to the slurry at a dropping rate of 1 mL / min, stir at 500 rpm until the dropping is finished, homogenize at 1000 bar for 2 min each time, stir at 300 rpm for 1 h, let stand at room temperature for 26 h, and filter through a 200 mesh screen to obtain the final product.

[0092] The total amount of graphene-coated carbon nanotube powder in step Z2 is 15wt% of the slurry; the shear dispersion refers to stirring at 3000rpm for 10min, then stirring at 8000rpm for 30min, and finally setting the ultrasonic frequency to 45kHz, the ultrasonic power to 300W, and sonicating for 20min.

[0093] The preparation method of graphene-coated carbon nanotube powder in step Z2 includes the following steps:

[0094] Step Y1: Mix graphene oxide, carboxylated carbon nanotubes, and deionized water in a mass ratio of 1:3:100, set the ultrasonic frequency to 40kHz and the ultrasonic power to 350W, and sonicate for 30 minutes to obtain a suspension.

[0095] Step Y2: KH-550 and the suspension are mixed at a mass ratio of 1:66.5-67.1 and stirred in an oil bath at 80℃ and 900rpm for 3.5h to obtain the reaction solution;

[0096] Step Y3: Centrifuge the reaction solution to collect the precipitate, wash it three times with anhydrous ethanol, and dry it under vacuum at 60℃ for 28 hours to obtain the final product.

[0097] Step 5 refers to the finishing process of immersing the conductive nylon fabric in an aqueous solution of amino silicone oil containing 6 wt% amino silicone oil until the liquid ratio reaches 80%, baking at 110°C for 3 minutes, and then heat-setting at 160°C for 30 seconds.

[0098] The modified nylon fabric is used to prepare underwear and nylon cloth.

[0099] Example 4

[0100] A method for preparing a highly elastic, antistatic modified nylon fabric, the method comprising the following steps:

[0101] Step 1: Immerse the nylon fabric in a non-ionic surfactant solution, wash with water until neutral, and dehydrate to obtain the treated nylon fabric.

[0102] Step 2: Immerse the treated nylon fabric in a benzyl alcohol solution to swell, then dry it to obtain the swollen nylon fabric.

[0103] Step 3: Mix the swollen nylon fabric with the polyetheramine solution, wash with acetone to remove unreacted monomers, and dry to obtain the modified nylon fabric.

[0104] Step 4: Mix the modified nylon fabric with the conductive paste, sonicate, perform gradient drying, and plasma treatment to obtain the conductive nylon fabric.

[0105] Step 5: Perform post-treatment on the conductive nylon fabric to obtain the final product.

[0106] The nonionic surfactant solution mentioned in step one is an aqueous solution containing 1.7 wt% Triton X-100; the dehydration refers to dehydration to a water content of 18 wt%.

[0107] The benzaldehyde content in the benzaldehyde solution in step two is 42 wt%; the swelling refers to swelling by constant temperature oscillation at 51°C for 36 min at an oscillation frequency of 75 rpm; the drying refers to drying with hot air circulation at 80°C until the moisture content is less than 3%.

[0108] The mass ratio of the swollen nylon fabric to the polyetheramine solution in step three is 1:19.4; the polyetheramine solution is obtained by mixing polyetheramine, HDI trimer, and 68-74 wt% ethanol solution in a mass ratio of 1.37:2.6:8.9; the mixing refers to adjusting the pH to 8.5 with triethylamine, shaking at 43°C for 2.8 h, pre-drying at 80°C for 37 min after shaking, and then heat curing at 120°C for 48 min; the drying temperature is 80°C.

[0109] The mass ratio of the modified nylon fabric to the conductive paste in step four is 1:15; the ultrasonication refers to setting the ultrasonic frequency to 46kHz, the ultrasonic power to 170W, the ultrasonic temperature to 52℃, and ultrasonication for 38 minutes; the gradient drying refers to drying at 60℃ for 25 minutes first, and then drying at 100℃ for 15.5 minutes; the plasma treatment refers to setting the power to 260W, the processing speed to 3.3m / min, introducing 21wt% oxygen and the remainder argon, and plasma treatment for 4.5 minutes.

[0110] The preparation method of the conductive paste described in step four includes the following steps:

[0111] Step Z1: Polyvinylpyrrolidone and deionized water were stirred at 48°C for 32 min to prepare a polyvinylpyrrolidone solution with a total polyvinylpyrrolidone content of 1.8 wt%.

[0112] Step Z2: Add graphene-coated carbon nanotube powder to polyvinylpyrrolidone solution, stir at 680 rpm for 26 min, then shear disperse, cool, and obtain slurry;

[0113] Step Z3: Add 5.7 wt% of waterborne polyurethane to the slurry at a dropping rate of 1.2 mL / min, stir at 550 rpm until the dropping is finished, homogenize at 1100 bar for 2.5 min each time, stir at 320 rpm for 1.1 h, let stand at room temperature for 27 h, and filter through a 200 mesh screen to obtain the final product.

[0114] The total amount of graphene-coated carbon nanotube powder in step Z2 is 15.3 wt% of the slurry; the shear dispersion refers to stirring at 3300 rpm for 11 min, then stirring at 8500 rpm for 34 min, and finally setting the ultrasonic frequency to 46 kHz, the ultrasonic power to 310 W, and sonicating for 21 min.

[0115] The preparation method of graphene-coated carbon nanotube powder in step Z2 includes the following steps:

[0116] Step Y1: Mix graphene oxide, carboxylated carbon nanotubes, and deionized water in a mass ratio of 1:3.1:107, set the ultrasonic frequency to 48kHz, the ultrasonic power to 360W, and sonicate for 35 minutes to obtain a suspension.

[0117] Step Y2: KH-550 and the suspension are mixed at a mass ratio of 1:67 and stirred in an oil bath at 80℃ and 940rpm for 3.7h to obtain the reaction solution;

[0118] Step Y3: Centrifuge the reaction solution to collect the precipitate, wash it three times with anhydrous ethanol, and dry it under vacuum at 60℃ for 30 hours to obtain the final product.

[0119] The finishing process described in step five refers to immersing the conductive-treated nylon fabric in an aqueous solution of amino silicone oil containing 6.5 wt% amino silicone oil until the liquid yield is 81%, baking at 112°C for 3.5 min, and then heat-setting at 161°C for 31 s.

[0120] The modified nylon fabric is used to prepare underwear and nylon cloth.

[0121] Example 5

[0122] A method for preparing a highly elastic, antistatic modified nylon fabric, the method comprising the following steps:

[0123] Step 1: Immerse the nylon fabric in a non-ionic surfactant solution, wash with water until neutral, and dehydrate to obtain the treated nylon fabric.

[0124] Step 2: Immerse the treated nylon fabric in a benzyl alcohol solution to swell, then dry it to obtain the swollen nylon fabric.

[0125] Step 3: Mix the swollen nylon fabric with the polyetheramine solution, wash with acetone to remove unreacted monomers, and dry to obtain the modified nylon fabric.

[0126] Step 4: Mix the modified nylon fabric with the conductive paste, sonicate, perform gradient drying, and plasma treatment to obtain the conductive nylon fabric.

[0127] Step 5: Perform post-treatment on the conductive nylon fabric to obtain the final product.

[0128] The nonionic surfactant solution mentioned in step one is an aqueous solution containing 2 wt% Triton X-100; the dehydration refers to dehydration to a water content of 20 wt%.

[0129] The benzaldehyde content in the benzaldehyde solution in step two is 45 wt%; the swelling refers to swelling by constant temperature oscillation at 52°C for 40 min at an oscillation frequency of 80 rpm; the drying refers to drying by hot air circulation at 80°C until the moisture content is less than 3%.

[0130] The mass ratio of the swollen nylon fabric to the polyetheramine solution in step three is 1:20; the polyetheramine solution is obtained by mixing polyetheramine, HDI trimer, and 74wt% ethanol solution in a mass ratio of 1.4:3:9; the mixing refers to adjusting the pH to 8.5 with triethylamine, shaking at 44℃ for 3 hours, pre-drying at 80℃ for 40 minutes after shaking, and then heat curing at 120℃ for 50 minutes; the drying temperature is 80℃.

[0131] The mass ratio of the modified nylon fabric to the conductive paste in step four is 1:16; the ultrasonication refers to setting the ultrasonic frequency to 50kHz, the ultrasonic power to 200W, the ultrasonic temperature to 55℃, and ultrasonication for 40 minutes; the gradient drying refers to drying at 60℃ for 26 minutes first, and then drying at 100℃ for 16 minutes; the plasma treatment refers to setting the power to 300W, the processing speed to 4m / min, introducing 22wt% oxygen and the remainder argon, and plasma treatment for 5 minutes.

[0132] The preparation method of the conductive paste described in step four includes the following steps:

[0133] Step Z1: Polyvinylpyrrolidone and deionized water are stirred at 50°C for 35 min to prepare a polyvinylpyrrolidone solution with a total polyvinylpyrrolidone content of 2 wt%.

[0134] Step Z2: Add graphene-coated carbon nanotube powder to polyvinylpyrrolidone solution, stir at 700 rpm for 30 min, then shear dispersion, cool, and obtain slurry;

[0135] Step Z3: Add 6 wt% of waterborne polyurethane to the slurry at a dropping rate of 0.15 mL / min, stir at 600 rpm until the dropping is finished, homogenize at 1200 bar for 3 min each time, stir at 350 rpm for 1.2 h, let stand at room temperature for 28 h, and filter through a 200 mesh screen to obtain the final product.

[0136] The total amount of graphene-coated carbon nanotube powder in step Z2 is 16 wt% of the slurry; the shear dispersion refers to stirring at 3500 rpm for 12 min, then stirring at 9000 rpm for 35 min, and finally setting the ultrasonic frequency to 50 kHz, the ultrasonic power to 350 W, and sonicating for 22 min.

[0137] The preparation method of graphene-coated carbon nanotube powder in step Z2 includes the following steps:

[0138] Step Y1: Mix graphene oxide, carboxylated carbon nanotubes, and deionized water in a mass ratio of 1:3.2:110, set the ultrasonic frequency to 50kHz, the ultrasonic power to 400W, and sonicate for 40 minutes to obtain a suspension.

[0139] Step Y2: KH-550 and the suspension are mixed at a mass ratio of 1:67.1 and stirred in an oil bath at 80°C and 1000 rpm for 4 hours to obtain the reaction solution.

[0140] Step Y3: Centrifuge the reaction solution to collect the precipitate, wash it three times with anhydrous ethanol, and dry it under vacuum at 60℃ for 32 hours to obtain the final product.

[0141] Step 5 refers to the finishing process of immersing the conductive nylon fabric in an amino silicone oil aqueous solution containing 7wt% amino silicone oil until the roll-off rate is 82%, baking at 115℃ for 4 minutes, and then heat-setting at 162℃ for 35 seconds.

[0142] The modified nylon fabric is used to prepare underwear and nylon cloth.

[0143] Example 6

[0144] Based on Example 3, the graphene-coated carbon nanotube powder was removed and replaced with an equal weight of graphene oxide, while other conditions remained the same as in Example 3.

[0145] Example 7

[0146] Based on Example 3, the graphene-coated carbon nanotube powder was removed and replaced with an equal weight of hydroxylated carbon nanotubes, while other conditions remained the same as in Example 3.

[0147] Example 8

[0148] Based on Example 3, the graphene-coated carbon nanotube powder was removed and replaced with equal weights of graphene oxide and hydroxylated carbon nanotubes, with a mass ratio of graphene oxide to hydroxylated carbon nanotubes of 1:3.

[0149] Comparative Example 1

[0150] Based on Example 3, while keeping other conditions the same, the preparation method of the modified nylon fabric was changed to the following steps:

[0151] Step 1: Immerse the nylon fabric in a non-ionic surfactant solution, wash with water until neutral, and dehydrate to obtain the treated nylon fabric.

[0152] Step 2: Mix the treated nylon fabric with the polyetheramine solution, wash with acetone to remove unreacted monomers, and dry to obtain the modified nylon fabric.

[0153] Step 3: Mix the modified nylon fabric with the conductive paste, sonicate, then perform gradient drying and plasma treatment to obtain the conductive nylon fabric.

[0154] Step 4: Perform post-treatment on the conductive nylon fabric to obtain the final product.

[0155] Comparative Example 2

[0156] Based on Example 3, while keeping other conditions the same, the preparation method of the modified nylon fabric was changed to the following steps:

[0157] Step 1: Immerse the nylon fabric in a non-ionic surfactant solution, wash with water until neutral, and dehydrate to obtain the treated nylon fabric.

[0158] Step 2: Immerse the treated nylon fabric in a benzyl alcohol solution to swell, then dry it to obtain the swollen nylon fabric.

[0159] Step 3: Mix the swollen nylon fabric with the conductive paste, sonicate, perform gradient drying, and plasma treatment to obtain the conductive nylon fabric.

[0160] Step 4: Perform post-treatment on the conductive nylon fabric to obtain the final product.

[0161] Comparative Example 3

[0162] Based on Example 3, while keeping other conditions the same, the preparation method of the modified nylon fabric was changed to the following steps:

[0163] Step 1: Immerse the nylon fabric in a non-ionic surfactant solution, wash with water until neutral, and dehydrate to obtain the treated nylon fabric.

[0164] Step 2: Immerse the treated nylon fabric in a benzyl alcohol solution to swell, then dry it to obtain the swollen nylon fabric.

[0165] Step 3: Mix the swollen nylon fabric with the conductive paste, sonicate, perform gradient drying, and plasma treatment to obtain the conductive nylon fabric.

[0166] Step 4: Mix the conductive treated nylon fabric with the polyetheramine solution, wash with acetone to remove unreacted monomers, and dry to obtain the modified nylon fabric.

[0167] Step 5: Perform finishing on the modified nylon fabric to obtain the final product.

[0168] Comparative Example 4

[0169] Based on Example 3, while keeping other conditions consistent, the preparation method of graphene-coated carbon nanotube powder was changed to the following steps:

[0170] Step Y1: Mix graphene oxide, carboxylated carbon nanotubes, and deionized water in a mass ratio of 1:3:100, set the ultrasonic frequency to 40kHz and the ultrasonic power to 350W, and sonicate for 30 minutes to obtain a suspension.

[0171] Step Y2: Centrifuge the suspension to collect the precipitate, wash it three times with anhydrous ethanol, and dry it under vacuum at 60℃ for 28 hours to obtain the final product.

[0172] To better test the elasticity and antistatic properties of the fabric in practical applications, modified nylon fabrics prepared in Examples 1-8 and Comparative Examples 1-4 were used as samples. The recovery rate of the samples after holding at a tensile elongation of 10% for 1 hour was measured according to FZ / T 01034-2008. The surface resistance of the samples was measured according to GB / T12703.4-2010. Three sets of parallel tests were performed for each measurement, and the average test results were recorded in Table 1 below.

[0173] Table 1

[0174]

[0175]

[0176] As shown in Table 1, the modified nylon fabric prepared in the embodiments of the present invention has good elasticity and antistatic properties.

[0177] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Although the present invention has been disclosed above with reference to preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some modifications or alterations to the above-disclosed technical content to create equivalent embodiments without departing from the scope of the present invention. Any indirect modifications, equivalent changes, and alterations made to the above embodiments based on the technical essence of the present invention without departing from the scope of the present invention shall still fall within the scope of the present invention.

Claims

1. A method for preparing a highly elastic, antistatic modified nylon fabric, characterized in that: The preparation method includes the following steps: Step 1: Immerse the nylon fabric in a non-ionic surfactant solution, wash with water until neutral, and dehydrate to obtain the treated nylon fabric. Step 2: Immerse the treated nylon fabric in a benzyl alcohol solution to swell, then dry it to obtain the swollen nylon fabric. Step 3: Mix the swollen nylon fabric with the polyetheramine solution, wash with acetone to remove unreacted monomers, and dry to obtain the modified nylon fabric. Step 4: Mix the modified nylon fabric with the conductive paste, sonicate, perform gradient drying, and plasma treatment to obtain the conductive nylon fabric. Step 5: Perform finishing on the conductive nylon fabric to obtain the final product. The mass ratio of the swollen nylon fabric to the polyetheramine solution described in step three is 1:18-20; The polyetheramine solution is obtained by mixing polyetheramine, HDI trimer, and 68-74 wt% ethanol solution in a mass ratio of 1.2-1.4:2-3:8.6-9. The mixing of the polyetheramine solution refers to adjusting the pH to 8.3-8.5 with triethylamine, shaking at 40-44℃ for 2-3 hours, pre-drying at 80℃ for 30-40 minutes after shaking, and then heat-curing at 120℃ for 40-50 minutes. The drying temperature is 80℃. The preparation method of the conductive paste described in step four includes the following steps: Step Z1: Polyvinylpyrrolidone and deionized water are stirred at 40-50℃ for 25-35 min to prepare a polyvinylpyrrolidone solution with a total polyvinylpyrrolidone content of 1-2 wt%. Step Z2: Add graphene-coated carbon nanotube powder to a polyvinylpyrrolidone solution, stir at 500-700 rpm for 20-30 min, then shear and disperse, cool, and obtain a slurry; Step Z3: Add 5-6 wt% of waterborne polyurethane to the slurry at a dropping rate of 0.5-1.5 mL / min, stir at 400-600 rpm until the dropping is finished, homogenize under high pressure at 800-1200 bar three times, each time for 1-3 min, then stir at 250-350 rpm for 0.8-1.2 h, let stand at room temperature for 24-28 h, and filter through a 200-mesh screen to obtain the final product. The preparation method of graphene-coated carbon nanotube powder in step Z2 includes the following steps: Step Y1: Mix graphene oxide, carboxylated carbon nanotubes, and deionized water in a mass ratio of 1:2.8-3.2:90-110, set the ultrasonic frequency to 30-50kHz, the ultrasonic power to 300-400W, and sonicate for 20-40 minutes to obtain a suspension. Step Y2: Mix KH-550 and the suspension at a mass ratio of 1:66.5-67.1, and stir in an oil bath at 80℃ and a speed of 800-1000rpm for 3-4 hours to obtain the reaction solution; Step Y3: Centrifuge the reaction solution to collect the precipitate, wash it three times with anhydrous ethanol, and dry it under vacuum at 60℃ for 24-32 hours to obtain the final product.

2. The method for preparing a highly elastic antistatic modified nylon fabric according to claim 1, characterized in that: The nonionic surfactant solution mentioned in step one is an aqueous solution containing 1-2 wt% Triton X-100; the dehydration refers to dehydration to a water content of 10-20 wt%.

3. The method for preparing a highly elastic antistatic modified nylon fabric according to claim 1, characterized in that: The benzaldehyde content in the benzaldehyde solution in step two is 35-45 wt%; the swelling refers to swelling by constant temperature oscillation at 48-52℃ for 30-40 minutes at an oscillation frequency of 60-80 rpm; the drying refers to drying with hot air circulation at 80℃ until the moisture content is less than 3%.

4. The method for preparing a highly elastic antistatic modified nylon fabric according to claim 1, characterized in that: The mass ratio of the modified nylon fabric to the conductive paste in step four is 1:12-16; the ultrasonication refers to setting the ultrasonic frequency to 40-50kHz, the ultrasonic power to 100-200W, the ultrasonic temperature to 45-55℃, and ultrasonication for 30-40 minutes; the gradient drying refers to drying at 60℃ for 20-26 minutes first, and then drying at 100℃ for 14-16 minutes; the plasma treatment refers to setting the power to 200-300W, the processing speed to 2-4m / min, introducing 18-22wt% oxygen and the remainder argon, and plasma treatment for 3-5 minutes.

5. The method for preparing a highly elastic antistatic modified nylon fabric according to claim 1, characterized in that: The total amount of graphene-coated carbon nanotube powder in step Z2 is 14-16 wt% of the slurry; the shear dispersion refers to stirring at 2500-3500 rpm for 8-12 min, then stirring at 7000-9000 rpm for 25-35 min, and finally setting the ultrasonic frequency to 40-50 kHz, the ultrasonic power to 250-350 W, and sonicating for 18-22 min.

6. The method for preparing a highly elastic antistatic modified nylon fabric according to claim 1, characterized in that: Step 5 refers to immersing the conductive-treated nylon fabric in an aqueous solution of amino silicone oil containing 5-7 wt% amino silicone oil until the roll-off rate is 78-82%, baking at 105-115℃ for 2-4 minutes, and then heat-setting at 158-162℃ for 25-35 seconds.

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