Anti-wrinkle and anti-pilling home wear fabric and preparation method thereof

Abstract

The present application relates to the technical field of high-performance acrylic fiber, and discloses an anti-wrinkle and anti-pilling home wear fabric and a preparation method thereof.The preparation method of the anti-wrinkle and anti-pilling home wear fabric comprises the following steps: preparing lignin micro-nano balls and modifying the same to obtain surface-modified lignin micro-nano balls; after the surface-modified lignin micro-nano balls are modified by a modifier, nano-silver is deposited on the surface of the surface-modified lignin micro-nano balls to obtain antibacterial modified lignin micro-nano balls; the antibacterial modified lignin micro-nano balls are loaded on surface-modified acrylic fiber to obtain loaded modified acrylic fiber; the loaded modified acrylic fiber is blended with cotton fiber, and then is knitted to obtain a base fabric; the base fabric is immersed in a polyurethane anti-wrinkle and anti-pilling finishing liquid, and then is baked to obtain the anti-wrinkle and anti-pilling home wear fabric.The anti-wrinkle and anti-pilling home wear fabric has the advantages of skin-friendly warmth, moisture absorption and air permeation, anti-pilling and anti-wrinkle, washing resistance, and long-lasting antibacterial property.

Description

Technical Field

[0001] This invention relates to the field of high-performance acrylic fiber technology, specifically to an anti-wrinkle and anti-pilling home wear fabric and its preparation method. Background Technology

[0002] As an essential part of modern people's daily leisure life, loungewear is receiving increasing attention. With the improvement of people's living standards, people have higher requirements for the comfort, warmth, safety, and health of loungewear fabrics.

[0003] Acrylic fiber, with its fluffy softness, strong warmth retention, wrinkle resistance, good weather resistance, and mildew and moth resistance, is often used in loungewear fabrics. However, acrylic fiber also suffers from poor moisture absorption and breathability, poor antibacterial properties, and a tendency to pill. In practical applications, acrylic fiber can be blended with other fibers. For example, cotton fiber has the advantages of being skin-friendly, warm, and breathable. Blending acrylic and cotton fibers can leverage these strengths and mitigate their weaknesses, improving the fabric's moisture absorption and breathability. However, cotton fiber wrinkles easily and has poor antibacterial properties. Therefore, solving the problems of wrinkle resistance, pilling resistance, and poor antibacterial properties in acrylic / cotton blended fabrics can provide wearers with a more comfortable, healthy, and safe wearing experience. Summary of the Invention

[0004] To address the aforementioned technical problems, this invention provides a method for preparing wrinkle-resistant and pilling-resistant loungewear fabric, comprising the following steps:

[0005] Step 1: Prepare lignin micro-nanospheres and modify them with acryloyl chloride to obtain surface-modified lignin micro-nanospheres;

[0006] Step 2: After the surface-modified lignin micro-nanospheres are modified with a modifier, nano-silver is deposited on their surface to obtain antibacterial modified lignin micro-nanospheres.

[0007] Step 3: Acrylic fibers are treated successively with diethylenetriamine aqueous solution and glutaraldehyde / ethanol solution to obtain surface-modified acrylic fibers; antibacterial modified lignin micro-nanospheres are loaded onto the surface-modified acrylic fibers to obtain loaded modified acrylic fibers.

[0008] Step 4: The modified acrylic fiber and cotton fiber are blended into a composite yarn, and the composite yarn is spun into a fabric through a knitting process to obtain the base fabric; the base fabric is dipped and rubbed twice in a polyurethane anti-wrinkle and anti-pilling finishing solution, and then baked to obtain an anti-wrinkle and anti-pilling home wear fabric.

[0009] Preferably, in step one, the preparation method of the surface-modified lignin micro / nanospheres is as follows: lignin is dissolved in a γ-valerol / water mixture to obtain a lignin solution with a concentration of 30-40 mg / mL; at 50°C, the lignin solution is mixed with deionized water at a volume ratio of (2-4):(8-16), ultrasonically treated for 10-20 min, dialyzed, and centrifuged to obtain lignin micro / nanospheres with an average particle size of 887-987 nm; the lignin micro / nanospheres are added to chloroform, stirred, and incubated at room temperature. Triethylamine was added, and the mixture was stirred in an ice-water bath for 10-15 minutes. Then, a 17.5% (w / w) acryloyl chloride / chloroform mixture was added dropwise over 1 hour at 0-5°C. The reaction was then carried out under a nitrogen atmosphere at room temperature with stirring for 40-50 hours. The pH of the reaction mixture was adjusted to 2. Finally, the reaction mixture was added to deionized water and stirred for 4-6 hours. After filtration, washing, and drying, surface-modified lignin micro / nanospheres were obtained. The mixture contained lignin micro / nanospheres, chloroform, triethylamine, and acryloyl chloride / chloroform. The mass ratio of the mixture is (5-8):(150-200):(7.4-11.8):(35.9-57.5); in the above process, lignin micro-nanospheres are prepared in the γ-valerol / water binary system, and then carbon-carbon double bonds are introduced on the lignin micro-nanospheres by reacting the acyl chloride in acryloyl chloride with the phenolic hydroxyl groups in lignin; preferably, in step two, the preparation method of the antibacterial modified lignin micro-nanospheres is as follows: the surface-modified lignin micro-nanospheres are added to ethanol, ultrasonicated, and heated to... At 60-70℃, a modifier and a 0.5% (w / w) azobisisobutyronitrile / ethanol mixed solution are added, and the mixture is stirred for 3-5 hours. After purification, composite modified lignin micro-nanospheres are obtained. The mass ratio of surface-modified lignin micro-nanospheres, ethanol, modifier, and azobisisobutyronitrile / ethanol mixed solution is (2.5-4.5):(150-200):(11.3-18.1):(20-30). The composite modified lignin micro-nanospheres are added to deionized water, and then a solution with a concentration of 0.A 6 g / mL solution of silver nitrate and sodium citrate was stirred and then subjected to a hydrothermal reaction at 120℃ for 100-140 min. After purification, antibacterial modified lignin micro-nanospheres were obtained. The ratio of the amount of composite modified lignin micro-nanospheres, deionized water, silver nitrate solution, and sodium citrate was 70 mg: 100 g: (5-7) mL: 3 g. In the above process, the carbon-carbon double bonds on the surface-modified lignin micro-nanospheres and the thiol groups on the modifier were combined through a click reaction, grafting the modifier onto the surface-modified lignin micro-nanospheres. The grafting of the modifier introduced abundant ammonia into the surface-modified lignin micro-nanospheres. The amino and thiol groups, along with Schiff base bonds, exhibit a strong affinity for silver ions, facilitating the capture of more silver ions. The amino group also acts as a silver ion reducing agent, synergistically promoting the formation of silver nanoparticles on lignin micro / nanospheres with sodium citrate. Therefore, using lignin micro / nanospheres as a carrier for silver nanoparticles, and immobilizing them through amino and thiol groups, allows for the slow release of silver. This approach enhances the long-lasting antibacterial ability of the antibacterial modified lignin micro / nanospheres while addressing the issue of cumulative toxicity of silver nanoparticles. Furthermore, the grafting of Schiff base bonds also contributes to improving the long-lasting antibacterial properties of the antibacterial modified lignin micro / nanospheres.

[0010] Preferably, in step two, the modifier is prepared by: adding 4-mercaptobenzaldehyde to N,N-dimethylformamide, sonicating, then adding 1,3-diamino-2-propanol, reacting at 80-100℃ for 8-10 h, purifying, and obtaining an intermediate product; wherein the mass ratio of 4-mercaptobenzaldehyde, N,N-dimethylformamide, and 1,3-diamino-2-propanol is (3.5-4.7):(200-300):(9-13.6); and then adding the intermediate product, 2,3-dimercaptosuccinic acid, p-toluenesulfonic acid, and cyclohexane in a ratio of (4.2-...). The mixtures were prepared in a mass ratio of (8.4): (1.8-3.6): (0.08-0.12): (8.5-16.5), and stirred at 200-210℃ for 2-3 hours under a nitrogen atmosphere. The mixture was then purified to obtain the modifier. In the above process, 4-mercaptobenzaldehyde and 1,3-diamino-2-propanol were combined through a Schiff base reaction to obtain an intermediate product containing thiol, Schiff base bond, amino group, and hydroxyl group. Next, the hydroxyl group of the intermediate product underwent an esterification reaction with the carboxyl groups at both ends of 2,3-dimercaptosuccinic acid to obtain a modifier containing thiol.

[0011] Preferably, in step three, the preparation method of the surface-modified acrylic fiber is as follows: The acrylic fiber is immersed in a 35% (w / w) diethylenetriamine aqueous solution with a solid-liquid ratio of 1:(15-25), stirred and immersed at 105-115℃ for 2-3 hours, then removed, washed, and dried to obtain pretreated acrylic fiber; the pretreated acrylic fiber is added to a 5% (w / w) glutaraldehyde / ethanol solution with a solid-liquid ratio of 1:(20-30), and immersed at 80-100℃. After soaking for 8-10 hours, remove, wash, and dry to obtain surface-modified acrylic fibers; preferably, in step three, the preparation method of the loaded modified acrylic fibers is as follows: antibacterial modified lignin micro-nanospheres are added to deionized water to form an antibacterial modified lignin micro-nanosphere dispersion with a concentration of 40-50 g / L; surface-modified acrylic fibers are added to the above-mentioned antibacterial modified lignin micro-nanosphere dispersion with a solid-liquid ratio of 1:(20-30), and soaked at 60-80℃ for 10-12 hours. After h, the fibers are removed, washed, and dried to obtain loaded modified acrylic fibers. During this process, the acrylic fibers are immersed in a diethylenetriamine aqueous solution. The cyano groups on the surface of the acrylic fibers react with the amino groups of the triethylenediamine, introducing abundant amino groups onto the surface of the acrylic fibers and improving their hydrophilic and hygroscopic properties. Next, glutaraldehyde is used as a crosslinking agent. The amino groups on the antibacterial modified lignin micro-nanospheres and pretreated acrylic fibers react with glutaraldehyde to generate Schiff base bonds, firmly attaching the antibacterial modified lignin micro-nanospheres to the acrylic fibers in the form of chemical bonds. This prevents the antibacterial modified lignin micro-nanospheres from falling off and also roughens the surface of the acrylic fibers, enhancing the cohesion between fibers, thereby improving the wrinkle resistance and pilling resistance of the acrylic fibers. Preferably, in step four, the English count of the composite yarn is 30-40S, and the mass ratio of loaded modified acrylic fibers to cotton fibers in the composite yarn is 1:(0.5-0.8); the basis weight of the base fabric is 80-100 g / m². 2 Preferably, in step four, the base fabric has a liquid retention rate of 70-80% when impregnated in the polyurethane anti-wrinkle and anti-pilling finishing liquid; baking conditions: baking at 145-155℃ for 2-4 minutes.

[0012] Preferably, in step four, the preparation method of the polyurethane anti-wrinkle and anti-pilling finishing liquid is as follows: polyethylene glycol, isoflurane diisocyanate, dimethylolpropionic acid, and N,N-dimethylacetamide are mixed and stirred, then dibutyltin dilaurate is added, and the mixture is reacted at 86-90℃ for 2-3 hours to obtain a prepolymer; the temperature is lowered to 60-64℃, and 2-chloro-4,6-diamino-1,3,5-triazine and N-methyldiethanolamine are added to the prepolymer, and the mixture is reacted at 68-72℃ for 2.5-3.5 hours, and then... 1,6-Dibromohexane was added, and the reaction continued for 1.5-2.5 hours. Triethylamine was then added and the reaction was continued for 40-50 minutes. The mixture was then rotary evaporated, and distilled water was added to obtain a polyurethane anti-wrinkle and anti-pilling finishing solution with a concentration of 20-40 g / L. The mass ratio of polyethylene glycol, isoflurane diisocyanate, dimethylolpropionic acid, N,N-dimethylacetamide, dibutyltin dilaurate, 2-chloro-4,6-diamino-1,3,5-triazine, N-methyldiethanolamine, 1,6-dibromohexane, and triethylamine was (12-18). (8.9-13.3): (2.6-3.9): (9.3-13.9): (0.2-0.5): (0.7-1.5): (0.4-0.8): (0.4-0.8): (2-3); In the above process, polyethylene glycol and isoflurane diisocyanate are polymerized under the catalysis of dibutyltin dilaurate to obtain a prepolymer. The isocyanate groups in the prepolymer react with the amino groups of 2-chloro-4,6-diamino-1,3,5-triazine and N-methyldiethanolamine, and then... The quaternization reaction between 1,6-dibromohexane and N-methyldiethanolamine introduces a halotriazine ring and a quaternary ammonium salt structure into the polyurethane chain. The halogen atoms on the halotriazine ring can replace the hydroxyl groups on cotton fibers and loaded modified acrylic fibers, enabling strong chemical cross-linking between polyurethane and cotton fibers, as well as loaded modified acrylic fibers, thereby improving the anti-wrinkle and anti-pilling properties of the fabric. In addition, the introduction of the quaternary ammonium salt structure into the polyurethane chain gives the polyurethane anti-wrinkle and anti-pilling finishing liquid a lasting antibacterial property, thus endowing the fabric with better antibacterial properties.

[0013] The wrinkle-resistant and pilling-resistant loungewear fabric is prepared using the aforementioned method.

[0014] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0015] 1. The intermediate product of this invention undergoes an esterification reaction with 2,3-dimercaptosuccinic acid to generate a modifier. The modifier is then used to modify lignin micro-nanospheres, introducing amino and thiol groups to serve as a carrier for silver nanospheres. This enables the generation and sustained release of silver nanospheres, enhancing the long-lasting antibacterial ability of the antibacterial modified lignin micro-nanospheres while solving the problem of cumulative toxicity of silver nanospheres. This makes the process more environmentally friendly and safer. Furthermore, the generation of silver nanospheres increases the surface roughness of the lignin micro-nanospheres. In addition, the synergistic effect of silver nanospheres with Schiff base bonds enhances the antibacterial properties of the antibacterial modified lignin micro-nanospheres.

[0016] 2. This invention pretreats acrylic fibers with triethylenediamine to improve their hydrophilic and moisture-absorbing properties, and then grafts antibacterial modified lignin micro-nanospheres onto the acrylic fibers in the form of chemical bonds, giving the acrylic fibers long-lasting antibacterial properties and improving their anti-wrinkle and anti-pilling properties.

[0017] 3. This invention uses a blend of cotton fiber and modified acrylic fiber to form a base fabric, which maximizes the advantages and minimizes the disadvantages, giving the base fabric the advantages of being skin-friendly and warm, moisture-wicking and breathable, anti-pilling and wrinkle-resistant, and long-lasting antibacterial. Then, the base fabric is finished with a polyurethane anti-pilling and wrinkle-resistant finishing liquid to obtain an anti-pilling and wrinkle-resistant loungewear fabric. The presence of quaternary ammonium salts and halotriazine rings in the polyurethane anti-pilling and wrinkle-resistant finishing liquid can cross-link with cotton fiber and modified acrylic fiber through chemical bonds, giving the loungewear fabric better anti-pilling and wrinkle-resistant properties and long-lasting antibacterial properties.

[0018] Therefore, this invention combines the grafting modification of acrylic fibers with finishing with polyurethane anti-wrinkle and anti-pilling finishing liquid to obtain an anti-pilling and anti-wrinkle homewear fabric with skin-friendly warmth, moisture absorption and breathability, and long-lasting antibacterial properties, providing wearers with a more comfortable, healthy and safe wearing experience. Attached Figure Description

[0019] Figure 1 This is a comparison chart of the fold recovery angle test results of the wrinkle-resistant and pilling-resistant home wear fabrics prepared in Examples 3-5 and Comparative Examples 1-3 of the present invention;

[0020] Figure 2 This is a comparison chart of the Staphylococcus aureus inhibition rate (0 washes and 50 washes) of the anti-wrinkle and anti-pilling home wear fabrics prepared in Examples 3-5 and Comparative Examples 1-3 of the present invention. Detailed Implementation

[0021] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. All other embodiments obtained by those skilled in the art based on the embodiments of the present invention without creative effort are within the scope of protection of the present invention.

[0022] Example 1

[0023] This embodiment discloses a method for preparing a modifier, comprising the following steps: 4.1g of 4-mercaptobenzaldehyde is added to 250g of N,N-dimethylformamide and ultrasonically treated for 45min. Then, 11.3g of 1,3-diamino-2-propanol is added, and the mixture is reacted at 90℃ for 9h. After the reaction is completed, the mixture is cooled to room temperature, the solvent is evaporated, and the resulting solid product is washed with deionized water and dried to obtain an intermediate product. 6.3g of the intermediate product, 2.7g of 2,3-dimercaptosuccinic acid, 0.1g of p-toluenesulfonic acid, and 12.5g of cyclohexane are mixed and stirred at 205℃ for 2.5h under a nitrogen atmosphere. After the reaction is completed, the mixture is cooled to room temperature, the product is dissolved in saturated sodium bicarbonate water, purified with deionized water, and rotary evaporated to obtain the modifier.

[0024] Example 2

[0025] This embodiment discloses a method for preparing a polyurethane anti-wrinkle and anti-pilling finishing liquid, comprising the following steps: mixing 15g of polyethylene glycol, 11.1g of isoflurane diisocyanate, 3.3g of dimethylolpropionic acid, and 11.6g of N,N-dimethylacetamide, stirring, and then adding 0.3g of dibutyltin dilaurate, reacting at 88°C for 2.5h to obtain a prepolymer; cooling to 62°C, and adding 1.1g of 2-chloro-4,6-diamino-1,3,5-triazine and 0.6g of N-methyldiethanolamine to the prepolymer, reacting at 70°C for 3h, then adding 0.6g of 1,6-dibromohexane, continuing the reaction for 2h, adding 2.5g of triethylamine and reacting for 45min, removing the solvent by rotary evaporation, and then adding distilled water to obtain a polyurethane anti-wrinkle and anti-pilling finishing liquid with a concentration of 30g / L.

[0026] Example 3

[0027] This embodiment discloses a method for preparing wrinkle-resistant and pilling-resistant loungewear fabric, including the following steps:

[0028] Step 1: Dissolve lignin in a γ-valerol / water mixture at a volume ratio of 9:1 to obtain a lignin solution with a concentration of 30 mg / mL. Add 2 mL of the lignin solution rapidly to 8 mL of deionized water at 50 °C, sonicate for 10 min, then transfer the resulting suspension to a dialysis bag (molecular weight cutoff of 1000), soak in deionized water for 36 h, and centrifuge to obtain lignin micro / nanospheres with an average particle size of 887 nm. Add 5 g of lignin micro / nanospheres to 150 g of chloroform, stir for 40 min, and allow to stand at room temperature. Add 7.4 g of triethylamine, then stir in an ice-water bath for 10 min. Then add 35.9 g of a 17.5% acryloyl chloride / chloroform mixture dropwise at 0 °C over 1 h. Then stir the mixture at room temperature under a nitrogen atmosphere for 40 h. Adjust the pH of the reaction mixture to 2 with a 1 mol / L hydrochloric acid aqueous solution. Finally, add the reaction mixture to 1000 mL of deionized water and stir for 4 h. Filter the resulting mixture, wash the filter residue with deionized water and dry it to obtain surface-modified lignin micro-nanospheres.

[0029] Step 2: Add 2.5g of surface-modified lignin micro-nanospheres to 150g of ethanol, sonicate for 20min, heat to 60℃, then add 11.3g of modifier and 20g of azobisisobutyronitrile (0.5% by mass) azobisisobutyronitrile / ethanol mixed solution, stir and react for 3h. After the reaction is complete, filter, wash, and dry to obtain composite modified lignin micro-nanospheres; add 70mg of composite modified lignin micro-nanospheres to 100g of deionized water, then add 5mL of 0.6g / mL silver nitrate aqueous solution and 3g of sodium citrate, stir for 20min, then hydrothermally react at 120℃ for 100min. After the reaction is complete, centrifuge and freeze-dry to obtain antibacterial modified lignin micro-nanospheres;

[0030] Step 3: Immerse acrylic fibers in a 35% diethylenetriamine aqueous solution at a solid-liquid ratio of 1:15, stir and soak at 105℃ for 3 hours, then remove, rinse with deionized water until neutral, and dry to obtain pretreated acrylic fibers; add the pretreated acrylic fibers to a 5% glutaraldehyde / ethanol solution at a solid-liquid ratio of 1:20, soak at 80℃ for 10 hours, then remove, wash, and dry to obtain surface-modified acrylic fibers; add antibacterial modified lignin micro-nanospheres to deionized water to form an antibacterial modified lignin micro-nanosphere dispersion at a concentration of 40 g / L; add the surface-modified acrylic fibers to the above antibacterial modified lignin micro-nanosphere dispersion at a solid-liquid ratio of 1:20, soak at 60℃ for 12 hours, then remove, wash, and dry to obtain loaded modified acrylic fibers;

[0031] Step 4: Blend the modified acrylic fiber and cotton fiber at a mass ratio of 1:0.5 to form a composite yarn with a yarn count of 30S (English count). Then, knit the composite yarn into a fabric with a weight of 80 g / m². 2 The base fabric was dipped and rolled twice in a polyurethane anti-wrinkle and anti-pilling finishing solution, and then baked to obtain an anti-wrinkle and anti-pilling home wear fabric; wherein, the liquid retention rate of the base fabric in the polyurethane anti-wrinkle and anti-pilling finishing solution was 70%; baking conditions: baking at 145℃ for 4 minutes.

[0032] Example 4

[0033] This embodiment discloses a method for preparing wrinkle-resistant and pilling-resistant loungewear fabric, including the following steps:

[0034] Step 1: Dissolve lignin in a γ-valerol / water mixture at a volume ratio of 9:1 to obtain a lignin solution with a concentration of 40 mg / mL. Add 4 mL of the lignin solution rapidly to 16 mL of deionized water at 50 °C, sonicate for 20 min, then transfer the resulting suspension to a dialysis bag (molecular weight cutoff of 1000), soak in deionized water for 48 h, and centrifuge to obtain lignin micro / nanospheres with an average particle size of 987 nm. Add 8 g of the lignin micro / nanospheres to 200 g of chloroform, stir for 60 min, and allow to stand at room temperature. 11.8 g of triethylamine was added, and the mixture was stirred in an ice-water bath for 15 min. Then, 57.5 g of a 17.5% (w / w) acryloyl chloride / chloroform mixture was added dropwise at 5 °C over 1 h. The mixture was then stirred at room temperature under a nitrogen atmosphere for 50 h. The pH of the reaction mixture was then adjusted to 2 with a 1 mol / L hydrochloric acid aqueous solution. Finally, the reaction mixture was added to 1500 mL of deionized water and stirred for 6 h. The resulting mixture was then filtered, and the filter residue was washed with deionized water and dried to obtain surface-modified lignin micro-nanospheres.

[0035] Step 2: Add 4.5g of surface-modified lignin micro-nanospheres to 200g of ethanol, sonicate for 40min, heat to 70℃, then add 18.1g of modifier and 30g of azobisisobutyronitrile (0.5% by mass) azobisisobutyronitrile / ethanol mixed solution, stir and react for 5h. After the reaction is complete, filter, wash, and dry to obtain composite modified lignin micro-nanospheres; add 70mg of composite modified lignin micro-nanospheres to 100g of deionized water, then add 7mL of 0.6g / mL silver nitrate aqueous solution and 3g of sodium citrate, stir for 40min, then hydrothermally react at 120℃ for 140min. After the reaction is complete, centrifuge and freeze-dry to obtain antibacterial modified lignin micro-nanospheres;

[0036] Step 3: Immerse acrylic fibers in a 35% diethylenetriamine aqueous solution (solid-liquid ratio 1:25) at 115℃ for 2 hours with stirring. Remove the fibers, rinse with deionized water until neutral, and dry to obtain pretreated acrylic fibers. Add the pretreated acrylic fibers to a 5% glutaraldehyde / ethanol solution (solid-liquid ratio 1:30) at 100℃ for 8 hours. Remove the fibers, wash, and dry to obtain surface-modified acrylic fibers. Add antibacterial modified lignin micro / nanospheres to deionized water to form a 50 g / L antibacterial modified lignin micro / nanosphere dispersion. Add the surface-modified acrylic fibers to the above antibacterial modified lignin micro / nanosphere dispersion (solid-liquid ratio 1:30) at 80℃ for 10 hours. Remove the fibers, wash, and dry to obtain loaded modified acrylic fibers.

[0037] Step 4: Blend the modified acrylic fiber and cotton fiber at a mass ratio of 1:0.8 to form a composite yarn with a yarn count of 40S (English count). Then, knit the composite yarn into a fabric with a weight of 100 g / m². 2 The base fabric was dipped and rolled twice in a polyurethane anti-wrinkle and anti-pilling finishing solution, and then baked to obtain an anti-wrinkle and anti-pilling home wear fabric; wherein, the liquid-holding rate of the base fabric in the polyurethane anti-wrinkle and anti-pilling finishing solution was 80%; baking conditions: baking at 155℃ for 2 minutes.

[0038] Example 5

[0039] This embodiment discloses a method for preparing wrinkle-resistant and pilling-resistant loungewear fabric, including the following steps:

[0040] Step 1: Dissolve lignin in a γ-valerol / water mixture at a volume ratio of 9:1 to obtain a lignin solution with a concentration of 35 mg / mL. Add 3 mL of the lignin solution rapidly to 12 mL of deionized water at 50 °C, sonicate for 15 min, then transfer the resulting suspension to a dialysis bag (molecular weight cutoff of 1000), soak in deionized water for 42 h, and centrifuge to obtain lignin micro / nanospheres with an average particle size of 937 nm. Add 6.5 g of the lignin micro / nanospheres to 175 g of chloroform, stir for 50 min, and incubate at room temperature. Add 9.6 g of triethylamine, then stir in an ice-water bath for 12 min. Then add 46.7 g of a 17.5% acryloyl chloride / chloroform mixture dropwise at 3 °C over 1 h. Then stir the mixture at room temperature under a nitrogen atmosphere for 45 h. Adjust the pH of the reaction mixture to 2 with a 1 mol / L hydrochloric acid aqueous solution. Finally, add the reaction mixture to 1250 mL of deionized water and stir for 5 h. Filter the resulting mixture, wash the filter residue with deionized water and dry it to obtain surface-modified lignin micro-nanospheres.

[0041] Step 2: Add 3.5g of surface-modified lignin micro-nanospheres to 175g of ethanol, sonicate for 30min, heat to 65℃, then add 14.7g of modifier and 25g of azobisisobutyronitrile (0.5% by mass) azobisisobutyronitrile / ethanol mixed solution, stir and react for 4h. After the reaction is complete, filter, wash, and dry to obtain composite modified lignin micro-nanospheres; add 70mg of composite modified lignin micro-nanospheres to 100g of deionized water, then add 6mL of 0.6g / mL silver nitrate aqueous solution and 3g of sodium citrate, stir for 30min, then hydrothermally react at 120℃ for 120min. After the reaction is complete, centrifuge and freeze-dry to obtain antibacterial modified lignin micro-nanospheres;

[0042] Step 3: Immerse acrylic fibers in a 35% diethylenetriamine aqueous solution (solid-liquid ratio 1:20) at 110℃ for 2.5 hours with stirring. Remove the fibers, rinse with deionized water until neutral, and dry to obtain pretreated acrylic fibers. Add the pretreated acrylic fibers to a 5% glutaraldehyde / ethanol solution (solid-liquid ratio 1:25) at 90℃ for 9 hours. Remove the fibers, wash, and dry to obtain surface-modified acrylic fibers. Add antibacterial modified lignin micro / nanospheres to deionized water to form a 45 g / L antibacterial modified lignin micro / nanosphere dispersion. Add the surface-modified acrylic fibers to the above antibacterial modified lignin micro / nanosphere dispersion (solid-liquid ratio 1:25) at 70℃ for 11 hours. Remove the fibers, wash, and dry to obtain loaded modified acrylic fibers.

[0043] Step 4: Blend the modified acrylic fiber and cotton fiber at a mass ratio of 1:0.7 to form a composite yarn with a yarn count of 35S (English count). Then, knit the composite yarn into a fabric with a weight of 90 g / m². 2 The base fabric was dipped and rolled twice in a polyurethane anti-wrinkle and anti-pilling finishing solution, and then baked to obtain an anti-wrinkle and anti-pilling home wear fabric; wherein, the liquid-holding rate of the base fabric in the polyurethane anti-wrinkle and anti-pilling finishing solution was 75%; baking conditions: baking at 150℃ for 3 minutes.

[0044] Comparative Example 1

[0045] This comparative example discloses a method for preparing an anti-wrinkle and anti-pilling loungewear fabric, including the following steps:

[0046] Step 1: Dissolve lignin in a γ-valerol / water mixture at a volume ratio of 9:1 to obtain a lignin solution with a concentration of 35 mg / mL. Add 3 mL of the lignin solution rapidly to 12 mL of deionized water at 50 °C, sonicate for 15 min, then transfer the resulting suspension to a dialysis bag (molecular weight cutoff of 1000), soak in deionized water for 42 h, and centrifuge to obtain lignin micro / nanospheres with an average particle size of 937 nm. Add 6.5 g of the lignin micro / nanospheres to 175 g of chloroform, stir for 50 min, and incubate at room temperature. Add 9.6 g of triethylamine, then stir in an ice-water bath for 12 min. Then add 46.7 g of a 17.5% acryloyl chloride / chloroform mixture dropwise at 3 °C over 1 h. Then stir the mixture at room temperature under a nitrogen atmosphere for 45 h. Adjust the pH of the reaction mixture to 2 with a 1 mol / L hydrochloric acid aqueous solution. Finally, add the reaction mixture to 1250 mL of deionized water and stir for 5 h. Filter the resulting mixture, wash the filter residue with deionized water and dry it to obtain surface-modified lignin micro-nanospheres.

[0047] Step 2: Add 70mg of surface-modified lignin micro-nanospheres to 100g of deionized water, then add 6mL of 0.6g / mL silver nitrate aqueous solution and 3g of sodium citrate, stir for 30min, and then perform hydrothermal reaction at 120℃ for 120min. After the reaction is completed, centrifuge and freeze dry to obtain antibacterial modified lignin micro-nanospheres.

[0048] Step 3: Immerse acrylic fibers in a 35% diethylenetriamine aqueous solution (solid-liquid ratio 1:20) at 110℃ for 2.5 hours with stirring. Remove the fibers, rinse with deionized water until neutral, and dry to obtain pretreated acrylic fibers. Add the pretreated acrylic fibers to a 5% glutaraldehyde / ethanol solution (solid-liquid ratio 1:25) at 90℃ for 9 hours. Remove the fibers, wash, and dry to obtain surface-modified acrylic fibers. Add antibacterial modified lignin micro / nanospheres to deionized water to form a 45 g / L antibacterial modified lignin micro / nanosphere dispersion. Add the surface-modified acrylic fibers to the above antibacterial modified lignin micro / nanosphere dispersion (solid-liquid ratio 1:25) at 70℃ for 11 hours. Remove the fibers, wash, and dry to obtain loaded modified acrylic fibers.

[0049] Step 4: Blend the modified acrylic fiber and cotton fiber at a mass ratio of 1:0.7 to form a composite yarn with a yarn count of 35S (English count). Then, knit the composite yarn into a fabric with a weight of 90 g / m². 2The base fabric was dipped and rolled twice in a polyurethane anti-wrinkle and anti-pilling finishing solution, and then baked to obtain an anti-wrinkle and anti-pilling home wear fabric; wherein, the liquid-holding rate of the base fabric in the polyurethane anti-wrinkle and anti-pilling finishing solution was 75%; baking conditions: baking at 150℃ for 3 minutes.

[0050] Comparative Example 2

[0051] This comparative example discloses a method for preparing an anti-wrinkle and anti-pilling loungewear fabric, including the following steps:

[0052] Step 1: Immerse the acrylic fiber in a 35% diethylenetriamine aqueous solution with a solid-liquid ratio of 1:20. Stir and soak at 110℃ for 2.5 hours, then remove and rinse with deionized water until neutral. Dry to obtain pretreated acrylic fiber.

[0053] Step 2: Blend pretreated acrylic fibers and cotton fibers at a mass ratio of 1:0.7 to form a composite yarn with a yarn count of 35S (English count). Then, knit the composite yarn into a fabric with a weight of 90 g / m². 2 The base fabric was dipped and rolled twice in a polyurethane anti-wrinkle and anti-pilling finishing solution, and then baked to obtain an anti-wrinkle and anti-pilling home wear fabric; wherein, the liquid-holding rate of the base fabric in the polyurethane anti-wrinkle and anti-pilling finishing solution was 75%; baking conditions: baking at 150℃ for 3 minutes.

[0054] Comparative Example 3

[0055] This comparative example discloses a method for preparing an anti-wrinkle and anti-pilling loungewear fabric, including the following steps:

[0056] Step 1: Dissolve lignin in a γ-valerol / water mixture at a volume ratio of 9:1 to obtain a lignin solution with a concentration of 35 mg / mL. Add 3 mL of the lignin solution rapidly to 12 mL of deionized water at 50 °C, sonicate for 15 min, then transfer the resulting suspension to a dialysis bag (molecular weight cutoff of 1000), soak in deionized water for 42 h, and centrifuge to obtain lignin micro / nanospheres with an average particle size of 937 nm. Add 6.5 g of the lignin micro / nanospheres to 175 g of chloroform, stir for 50 min, and incubate at room temperature. Add 9.6 g of triethylamine, then stir in an ice-water bath for 12 min. Then add 46.7 g of a 17.5% acryloyl chloride / chloroform mixture dropwise at 3 °C over 1 h. Then stir the mixture at room temperature under a nitrogen atmosphere for 45 h. Adjust the pH of the reaction mixture to 2 with a 1 mol / L hydrochloric acid aqueous solution. Finally, add the reaction mixture to 1250 mL of deionized water and stir for 5 h. Filter the resulting mixture, wash the filter residue with deionized water and dry it to obtain surface-modified lignin micro-nanospheres.

[0057] Step 2: Add 3.5g of surface-modified lignin micro-nanospheres to 175g of ethanol, sonicate for 30min, heat to 65℃, then add 14.7g of modifier and 25g of azobisisobutyronitrile (0.5% by mass) azobisisobutyronitrile / ethanol mixed solution, stir and react for 4h. After the reaction is complete, filter, wash, and dry to obtain composite modified lignin micro-nanospheres; add 70mg of composite modified lignin micro-nanospheres to 100g of deionized water, then add 6mL of 0.6g / mL silver nitrate aqueous solution and 3g of sodium citrate, stir for 30min, then hydrothermally react at 120℃ for 120min. After the reaction is complete, centrifuge and freeze-dry to obtain antibacterial modified lignin micro-nanospheres;

[0058] Step 3: Immerse acrylic fibers in a 35% diethylenetriamine aqueous solution (solid-liquid ratio 1:20) at 110℃ for 2.5 hours with stirring. Remove the fibers, rinse with deionized water until neutral, and dry to obtain pretreated acrylic fibers. Add the pretreated acrylic fibers to a 5% glutaraldehyde / ethanol solution (solid-liquid ratio 1:25) at 90℃ for 9 hours. Remove the fibers, wash, and dry to obtain surface-modified acrylic fibers. Add antibacterial modified lignin micro / nanospheres to deionized water to form a 45 g / L antibacterial modified lignin micro / nanosphere dispersion. Add the surface-modified acrylic fibers to the above antibacterial modified lignin micro / nanosphere dispersion (solid-liquid ratio 1:25) at 70℃ for 11 hours. Remove the fibers, wash, and dry to obtain loaded modified acrylic fibers.

[0059] Step 4: Blend the modified acrylic fiber and cotton fiber at a mass ratio of 1:0.7 to form a composite yarn with a yarn count of 35S (English count). Then, knit the composite yarn into a fabric with a weight of 90 g / m². 2 The base fabric is a wrinkle-resistant and pill-resistant home wear fabric.

[0060] The modifiers and polyurethane anti-wrinkle and anti-pilling finishing liquids in Examples 3-5 and Comparative Examples 1-3 above use the modifier prepared in Example 1 and the polyurethane anti-wrinkle and anti-pilling finishing liquid prepared in Example 2.

[0061] In the above examples and comparative examples, polyethylene glycol (PEG), Mn=600g / mol, was from Jinan Qihang Chemical Technology Co., Ltd.; lignin, enzymatically hydrolyzed lignin (EHL) [hydroxyl content 1.87mmol (31PNMR), was from Laihe Biomass Co., Ltd., Hong Kong, China; acrylic fiber, with an average length of 38mm, was made from short-cut polyacrylonitrile filaments and came from Zhangjiagang Free Trade Zone Rimeda Fiber Trading Co., Ltd.; and cotton fiber, with a length of 38-39.7mm, was long-staple cotton from Xinjiang Uygur Autonomous Region.

[0062] Experimental Example

[0063] The performance of the wrinkle-resistant and pilling-resistant home wear fabrics prepared in Examples 3-5 and Comparative Examples 1-3 was tested.

[0064] I. Anti-pilling performance test: Tested according to standard GB / T4802.1-2008 Textiles - Pilling Test - Circular Trajectory Method;

[0065] II. Wrinkle resistance test: The test was conducted in accordance with the standard GB / T3819-1997 "Textiles - Determination of Crease Recovery - Recovery Angle Method";

[0066] III. Antibacterial performance test: The test standard GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles - Part 3: Shaking method" was adopted, and Staphylococcus aureus was selected as the test strain.

[0067] The test results are shown in Table 1:

[0068]

[0069] As can be seen from the test results in Table 1, the wrinkle-resistant and pilling-resistant home wear fabrics prepared in Examples 2-4 of the present invention have excellent wrinkle-resistant and pilling-resistant properties and long-lasting antibacterial properties. Comparison of Comparative Example 1 and Example 5 shows that modifying lignin micro-nanospheres with a modifier to introduce amino, thiol, and antibacterial Schiff base bonds achieves efficient generation and sustained release of nano-silver. Furthermore, the generation of nano-silver increases the surface roughness of the lignin micro-nanospheres and improves the surface roughness of the acrylic fibers, thereby enhancing the antibacterial, wrinkle-resistant, and anti-pilling properties of the acrylic fibers. Comparison of Comparative Example 2 and Example 5 shows that grafting antibacterial modified lignin micro-nanospheres onto acrylic fibers via chemical bonds gives the acrylic fibers durable antibacterial properties while improving their wrinkle-resistant and anti-pilling properties. Comparison of Comparative Example 3 and the examples shows that the presence of quaternary ammonium salts and halotriazine rings in the polyurethane anti-wrinkle and anti-pilling finishing liquid allows for cross-linking with cotton fibers and modified acrylic fibers through chemical bonds, giving the loungewear fabric better anti-pilling, wrinkle-resistant, and durable antibacterial properties.

[0070] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for preparing an anti-wrinkle and anti-pilling loungewear fabric, characterized in that, Includes the following steps: Step 1: Prepare lignin micro-nanospheres and modify them with acryloyl chloride to obtain surface-modified lignin micro-nanospheres; Step 2: After surface-modified lignin micro / nanospheres are treated with a modifier, nano-silver is deposited on their surface to obtain antibacterial modified lignin micro / nanospheres; wherein, the modifier is prepared by adding 4-mercaptobenzaldehyde to N,N-dimethylformamide, sonicating, then adding 1,3-diamino-2-propanol, reacting at 80-100℃ for 8-10 h, purifying, and obtaining an intermediate product; wherein, 4-mercaptobenzaldehyde, N,N-dimethylformamide, and 1... The mass ratio of 3-diamino-2-propanol was (3.5-4.7):(200-300):(9-13.6); the intermediate product, 2,3-dimercaptosuccinic acid, p-toluenesulfonic acid, and cyclohexane were mixed in a mass ratio of (4.2-8.4):(1.8-3.6):(0.08-0.12):(8.5-16.5), and the mixture was stirred and reacted at 200-210℃ for 2-3 hours under a nitrogen atmosphere. After purification, the modifier was obtained. Step 3: Acrylic fibers are treated successively with diethylenetriamine aqueous solution and glutaraldehyde / ethanol solution to obtain surface-modified acrylic fibers; antibacterial modified lignin micro-nanospheres are loaded onto the surface-modified acrylic fibers to obtain loaded modified acrylic fibers. Step 4: The modified acrylic fiber is blended with cotton fiber to form a composite yarn, which is then knitted to obtain a base fabric. The base fabric is then dipped and rubbed twice in a polyurethane anti-wrinkle and anti-pilling finishing solution, followed by baking to obtain an anti-wrinkle and anti-pilling loungewear fabric. The polyurethane anti-wrinkle and anti-pilling finishing solution is prepared as follows: polyethylene glycol, isoflurane diisocyanate, dimethylolpropionic acid, and N,N-dimethylacetamide are mixed and stirred. Then, dibutyltin dilaurate is added, and the mixture is reacted at 86-90℃ for 2-3 hours to obtain a prepolymer. The temperature is lowered to 60-64℃, and 2-chloro-4,6-diamino-1,3,5-triazine and N-methyldiethanolamine are added to the prepolymer. The mixture is reacted at 68-72℃ for 2.5-3.5 hours, and then 1,6-dibromohexane is added. Continue the reaction for 1.5-2.5 hours, add triethylamine and react for 40-50 minutes, rotary evaporate, and then add distilled water to obtain a polyurethane anti-wrinkle and anti-pilling finishing solution with a concentration of 20-40 g / L; wherein the mass ratio of polyethylene glycol, isoflurone diisocyanate, dimethylolpropionic acid, N,N-dimethylacetamide, dibutyltin dilaurate, 2-chloro-4,6-diamino-1,3,5-triazine, N-methyldiethanolamine, 1,6-dibromohexane, and triethylamine is (12-18):(8.9-13.3):(2.6-3.9):(9.3-13.9):(0.2-0.5):(0.7-1.5):(0.4-0.8):(0.4-0.8):(2-3).

2. The method for preparing the wrinkle-resistant and pilling-resistant loungewear fabric according to claim 1, characterized in that, In step one, the preparation method of the surface-modified lignin micro / nanospheres is as follows: lignin is dissolved in a γ-valerol / water mixture to obtain a lignin solution with a concentration of 30-40 mg / mL; at 50°C, the lignin solution is mixed with deionized water at a volume ratio of (2-4):(8-16), ultrasonically treated for 10-20 min, dialyzed, and centrifuged to obtain lignin micro / nanospheres with an average particle size of 887-987 nm; the lignin micro / nanospheres are added to chloroform, stirred, and triethylamine is added at room temperature, then stirred in an ice-water bath for 10-15 min. Then, a 17.5% (w / w) acryloyl chloride / chloroform mixture was added dropwise at 0-5℃ over 1 hour. The mixture was then stirred at room temperature under a nitrogen atmosphere for 40-50 hours. The pH of the reaction mixture was adjusted to 2. Finally, the reaction mixture was added to deionized water and stirred for 4-6 hours. The mixture was then filtered, washed, and dried to obtain surface-modified lignin micro / nanospheres. The mass ratio of lignin micro / nanospheres, chloroform, triethylamine, and acryloyl chloride / chloroform mixture was (5-8):(150-200):(7.4-11.8):(35.9-57.5).

3. The method for preparing the anti-wrinkle and anti-pilling loungewear fabric according to claim 1, characterized in that, In step two, the preparation method of the antibacterial modified lignin micro-nanospheres is as follows: Surface-modified lignin micro-nanospheres are added to ethanol, ultrasonicated, heated to 60-70℃, and then a modifier and a 0.5% (w / w) azobisisobutyronitrile / ethanol mixed solution are added. The mixture is stirred for 3-5 hours, purified, and the composite modified lignin micro-nanospheres are obtained. The mass ratio of surface-modified lignin micro-nanospheres, ethanol, modifier, and azobisisobutyronitrile / ethanol mixed solution is (2.5-4.5):(150-2). 00): (11.3-18.1): (20-30); The composite modified lignin micro-nanospheres were added to deionized water, and then silver nitrate aqueous solution with a concentration of 0.6 g / mL and sodium citrate were added. The mixture was stirred and then hydrothermally reacted at 120℃ for 100-140 min. After purification, antibacterial modified lignin micro-nanospheres were obtained. The ratio of the amount of composite modified lignin micro-nanospheres, deionized water, silver nitrate aqueous solution and sodium citrate was 70 mg: 100 g: (5-7) mL: 3 g.

4. The method for preparing the wrinkle-resistant and pilling-resistant loungewear fabric according to claim 1, characterized in that, In step three, the preparation method of the surface-modified acrylic fiber is as follows: the acrylic fiber is immersed in a 35% diethylenetriamine aqueous solution with a solid-liquid ratio of 1:(15-25), stirred and immersed at 105-115℃ for 2-3 hours, then removed, washed, and dried to obtain pretreated acrylic fiber; the pretreated acrylic fiber is added to a 5% glutaraldehyde / ethanol solution with a solid-liquid ratio of 1:(20-30), immersed at 80-100℃ for 8-10 hours, then removed, washed, and dried to obtain surface-modified acrylic fiber.

5. The method for preparing the wrinkle-resistant and pilling-resistant loungewear fabric according to claim 1, characterized in that, In step three, the method for preparing the loaded modified acrylic fiber is as follows: antibacterial modified lignin micro-nanospheres are added to deionized water to form an antibacterial modified lignin micro-nanosphere dispersion with a concentration of 40-50 g / L; surface-modified acrylic fiber is added to the above-mentioned antibacterial modified lignin micro-nanosphere dispersion with a solid-liquid ratio of 1:(20-30), and after soaking at 60-80℃ for 10-12 h, it is taken out, washed, and dried to obtain the loaded modified acrylic fiber.

6. The method for preparing the anti-wrinkle and anti-pilling loungewear fabric according to claim 1, characterized in that, In step four, the composite yarn has an English count of 30-40S, and the mass ratio of modified acrylic fiber to cotton fiber in the composite yarn is 1:(0.5-0.8); the base fabric has a basis weight of 80-100 g / m². 2 .

7. The method for preparing the wrinkle-resistant and pilling-resistant loungewear fabric according to claim 1, characterized in that, In step four, the base fabric is impregnated in polyurethane anti-wrinkle and anti-pilling finishing liquid with a liquid retention rate of 70-80%; baking conditions: baking at 145-155℃ for 2-4 minutes.

8. A wrinkle-resistant and pill-resistant loungewear fabric prepared by the method described in any one of claims 1-7.

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