Cool-feeling composite denim containing mint fibers and preparation method of cool-feeling composite denim

Abstract

The invention relates to the technical field of composite fabrics, and discloses cool composite denim containing mint fibers and a preparation method of the cool composite denim. The preparation method comprises the following steps: S1, preparing the lining fabric from the mint chinlon filaments; s2, cotton-viscose blended siro spinning 21-count yarn serves as warp yarn, blended fiber of natural mint fiber and cotton blended elastic yarn serves as weft yarn, denim fabric containing the mint fiber is prepared, and the denim fabric serves as surface fabric; the warp yarns and the weft yarns are interwoven in a three-up one-down right twill manner; s3, the inner layer fabric and the surface layer fabric are attached, stacked, aligned and sewn, and basic composite cloth is obtained; s4, the basic composite cloth is treated with the antibacterial finishing liquid, and the antibacterial modified composite cloth is obtained; and S5, treating the antibacterial modified composite fabric with the graphene finishing liquid to obtain the cool composite denim.

Description

Technical Field

[0001] The invention relates to the technical field of composite fabrics and discloses a cool composite denim containing mint fiber and a preparation method thereof. Background Art

[0002] Composite denim fabric has the advantages of good wear resistance, high elasticity and fashionable style, but traditional denim is thick and heavy, with poor breathability, which can easily make people feel stuffy and uncomfortable when worn in summer. It also has poor antibacterial properties, which may cause bacteria to breed, produce odor, skin infections and other problems.

[0003] Mint fiber is a new plant fiber with advantages such as antibacterial and deodorizing properties, a naturally cool feel, and excellent breathability. Its incorporation into composite denim fabrics can effectively improve comfort. To further enhance antibacterial properties, existing technologies use finishing agents to treat composite fabrics, but this often struggles to balance washability and breathability. Therefore, developing a cool composite denim fabric containing mint fiber that exhibits excellent antibacterial properties, washability, and breathability, as well as a method for its preparation, is of great significance. Summary of the Invention

[0004] The object of the present invention is to provide a cool composite denim containing mint fiber and a preparation method thereof, so as to solve the problems raised in the above background technology.

[0005] In order to solve the above technical problems, the present invention provides the following technical solution: a method for preparing a cool composite denim fabric containing mint fiber, comprising the following steps:

[0006] S1: The inner layer fabric was prepared with 40D / 36F mint nylon filament (Shandong Rare Technology Development Co., Ltd.);

[0007] S2: Referring to the prior art, a cotton-viscose blended siro-spun 21-count yarn was used as the warp yarn with a blending ratio of 70 / 30; a 1.21 / 40D natural mint fiber and a cotton blended stretch yarn were used as the weft yarn with a blending ratio of 60 / 40; a denim fabric containing mint fiber was prepared and used as the surface fabric; the warp yarns were interwoven with the weft yarns in a three-up-one-down right twill;

[0008] S3: Laminating the inner layer fabric and the outer layer fabric, aligning the layers, and sewing them using a nylon filament sewing thread through a multi-layer fabric quilting machine to obtain a basic composite fabric;

[0009] S4: treating the base composite fabric with an antibacterial finishing liquid to obtain an antibacterial modified composite fabric;

[0010] S5: The antibacterial modified composite fabric is treated with a graphene finishing liquid to obtain a cool composite denim fabric.

[0011] More optimally, the antibacterial finishing liquid comprises the following raw materials, calculated by weight: 10 to 12 parts of antibacterial agent, 100 parts of water, and 2 to 3 parts of glutaraldehyde;

[0012] The preparation of the antibacterial agent comprises the following steps: mixing mica powder, zinc oxide whiskers, ethanol and water, adjusting the pH to 3-5, adding coupling agent KH550, stirring at 50-70° C. for 2-4 hours, filtering and drying to obtain modified mica powder;

[0013] Add chitosan to acetic acid aqueous solution, add modified mica powder and stir evenly, add glutaraldehyde, stir and react at 50-60°C for 2-3 hours, filter, wash and dry to obtain modified chitosan; add butyl betaine hydrochloride, water, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide and N-hydroxysuccinimide, stir for 5-6 hours, filter, wash and dry to obtain an antibacterial agent.

[0014] More optimally, the modified mica powder comprises the following raw materials, calculated by weight: 40 to 50 parts of mica powder, 1 to 2 parts of zinc oxide whiskers, 60 to 80 parts of ethanol, 10 to 15 parts of water, and 0.2 to 0.6 parts of a coupling agent;

[0015] The antibacterial agent comprises the following raw materials, calculated by weight: 0.3-0.5 parts of chitosan, 0.1-0.2 parts of modified mica powder, 2-4 parts of glutaraldehyde, and 2-3 parts of butyl betaine hydrochloride.

[0016] More optimally, the specific steps of S4 are: mixing the base composite cloth and the antibacterial finishing liquid in a mass ratio of 1:30-50, immersing at a temperature of 50-60°C for 60-100 minutes, immersing and rolling, with a rolling rate of 80-90%, washing and drying to obtain the antibacterial modified composite cloth.

[0017] More optimally, the graphene finishing solution includes the following raw materials, calculated by weight: 15-20 parts of polymer-modified porous graphene, 100 parts of water, and 1-2 parts of glutaraldehyde;

[0018] The preparation of polymer-modified porous graphene includes the following steps: taking cinnamoyl chloride, pyridine, and menthol, stirring at 40-50° C. for 4-5 hours, adding 30-50 parts of water, extracting with 20-30 parts of ether four times, drying with anhydrous Na2SO4, removing the solvent, and further purifying by silica gel column chromatography with an eluent of v (petroleum ether: ethyl acetate) = 10:1 to obtain a double-bonded cooling agent;

[0019] Take double-bonded porous graphene, water, ethanol, and initiator, mix them evenly under ultrasonic mixing, add double-bonded cooling agent, acrylic acid, 2-hydroxyethyl acrylate, 2-acrylamide-2-methylpropanesulfonic acid, and acrylamide under nitrogen protection, stir and react at 75-78° C. for 8-12 hours, wash, filter, and dry to obtain polymer-modified porous graphene.

[0020] More optimally, the double-bonded cooling agent includes the following raw materials, calculated in parts by mass: 1 to 2 parts of cinnamoyl chloride, 5 to 6 parts of pyridine, and 1 to 2 parts of menthol; the polymer-modified porous graphene includes the following raw materials, calculated in parts by mass: 3 to 5 parts of double-bonded porous graphene, 0.1 to 0.3 parts of initiator, 0.4 to 0.6 parts of double-bonded cooling agent, 0.1 to 0.2 parts of acrylic acid, 0.3 to 0.4 parts of 2-hydroxyethyl acrylate, 0.05 to 0.1 parts of 2-acrylamide-2-methylpropanesulfonic acid, and 0.1 to 0.2 parts of acrylamide.

[0021] More optimally, the preparation method of double-bonded porous graphene is as follows: 10 to 15 parts of graphite are dispersed in 80 to 100 parts of a 50 wt% aqueous ethanol solution, ultrasonically dispersed for 2 to 3 hours, reacted at 160 to 165°C for 20 to 24 hours, washed, and dried to obtain porous graphene; added to a mixed solution of 30 to 50 parts of concentrated sulfuric acid and phosphoric acid, the volume ratio of concentrated sulfuric acid to phosphoric acid being 9:1, stirred and slowly added with 0.02 to 0.03 parts of KMnO4, stirred at 50 to 60°C for 16 to 20 hours, the obtained suspension is poured into 100 parts of cold water, 30% H2O2 is added to terminate the reaction, washed, and dried to obtain hydroxylated porous graphene;

[0022] Take 0.2-0.5 parts of hydroxylated porous graphene, add 40-50 parts of dichloromethane and 3-6 parts of triethylamine under nitrogen atmosphere, stir evenly, ultrasonicate at room temperature for 2-3 hours, add 10-15 parts of acryloyl chloride dropwise within 1 hour, stir at 40-50°C for 20-25 hours, then add 10-15 parts of ethanol, stir for 2-3 hours, wash, filter and dry to obtain double-bonded porous graphene.

[0023] More optimally, the specific steps of S5 are: mixing the antibacterial modified composite cloth and the graphene finishing liquid in a mass ratio of 1:30-50, immersing at a temperature of 50-60°C for 60-100 minutes, immersing and rolling once, with a rolling rate of 80-90%, baking at a temperature of 150-170°C for 5-10 minutes, washing, and drying to obtain a cool composite denim.

[0024] Compared with the existing technology, the present invention has the following beneficial effects: after the base composite cloth is prepared, it is treated with an antibacterial finishing liquid and a graphene finishing liquid in steps to obtain a cool composite denim cloth; compared with the one-step finishing method, the invention reduces the mutual interference between functional components, improves the uniformity, and fixes the cooling component on the surface of the fabric, further enhancing the cooling feeling;

[0025] The antibacterial agent raw materials in the antibacterial finishing liquid include mica powder modified with zinc oxide whiskers, chitosan, and butyl betaine hydrochloride; the mica powder has high thermal conductivity and can form a good thermal conduction path, thereby improving the cooling performance. After being modified with zinc oxide whiskers with a four-needle structure, the interlayer spacing is further expanded, thereby improving the thermal conductivity and the air permeability at the same time; in the antibacterial agent prepared by the present invention, the modified mica powder is combined with chitosan through glutaraldehyde to improve the antibacterial property and the dispersibility of the modified mica powder in the antibacterial finishing agent, and butyl betaine hydrochloride is grafted on the chitosan under the action of EDC and NHS, thereby optimizing the antibacterial property of the fabric and giving the fabric better softness, antistatic properties and hard water resistance, which are very helpful for improving the washability of the fabric; under the action of glutaraldehyde, the antibacterial agent combines with the abundant groups on the base composite cloth, thereby improving the bonding fastness and the washability. At the same time, since the modified mica powder is grafted into the antibacterial agent, it has good dispersibility and will not cause a decrease in air permeability;

[0026] Polymer-modified porous graphene is added to the graphene finishing liquid. Graphene has excellent antibacterial properties, and the porous graphene further improves its air permeability while improving its antibacterial properties. Menthol modified with cinnamoyl chloride is also added to the polymer, which has double bonds and is grafted onto the surface of the double-bonded porous graphene along with the polymer. The polymer also includes hydrophilic components such as acrylic acid, 2-hydroxyethyl acrylate, 2-acrylamide-2-methylpropanesulfonic acid, and acrylamide, which have good moisture absorption and perspiration properties, improve comfort, and can improve the dispersibility of graphene in water and its adhesion to fabrics. The presence of hydroxyl groups in the polymer-modified porous graphene allows for good bonding with fabrics under the action of glutaraldehyde.

[0027] In summary, after the basic composite cloth is prepared in this scheme, it is treated step by step with antibacterial finishing liquid and graphene finishing liquid to obtain a cool composite denim cloth; the components that provide antibacterial and cool properties are evenly dispersed on the fabric and have strong bonding force, and the fabric has good wash resistance without affecting breathability. DETAILED DESCRIPTION

[0028] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0029] It should be noted that the raw materials involved in the present invention are purchased from any manufacturer without any special restrictions, and illustratively include: ethanol (CAS: 64-17-5); mica powder (1250 mesh); zinc oxide whiskers (180314101638, four-needle zinc oxide whiskers, Kramar); KH550 (CAS: 919-30-2); chitosan (source leaf S11064); butyl betaine hydrochloride (CAS: 6249-56-5); cinnamoyl chloride (trans-3-phenylacryloyl chloride, CAS: 170 82-09-6); pyridine (CAS: 110-86-1); menthol (L-menthol, CAS: 2216-51-5); graphite (Yuanye S26651); dichloromethane (CAS: 75-09-2); acryloyl chloride (CAS: 814-68-6); initiator (BPO benzoyl peroxide); 2-acrylamido-2-methylpropanesulfonic acid (CAS: 15214-89-8); mint nylon filament (40D / 36F mint nylon filament, Shandong Rare Technology Development Co., Ltd.);

[0030] Unless otherwise specified, the following are parts by mass and mass ratios;

[0031] Preparation of a double-bond cooling agent: 2 parts of cinnamoyl chloride, 6 parts of pyridine, and 2 parts of menthol were stirred at 50°C for 5 hours, 50 parts of water were added, and the mixture was extracted four times with 30 parts of ether. The mixture was dried over anhydrous Na2SO4, the solvent was removed, and the mixture was further purified by silica gel column chromatography with an eluent of v (petroleum ether:ethyl acetate) = 10:1 to obtain a double-bond cooling agent.

[0032] Preparation of the basic composite fabric: The inner layer fabric is prepared using mint nylon filament yarn; cotton-viscose blended siro-spun 21-count yarn is used as the warp yarn with a blending ratio of 70 / 30; 1.21 / 40D natural mint fiber and cotton blended stretch yarn are used as the weft yarn with a blending ratio of 60 / 40; a denim fabric containing mint fiber is prepared as the surface fabric; the warp yarn and the weft yarn are interwoven in a three-up-one-down right twill; the inner layer fabric and the surface fabric are laminated and aligned, and sewn using nylon filament sewing thread on a multi-layer fabric quilting machine to obtain the basic composite fabric;

[0033] Example 1: S1: 45 parts of mica powder, 2 parts of zinc oxide whiskers, 80 parts of ethanol, and 10 parts of water were mixed, the pH was adjusted to 4, 0.5 parts of KH550 were added, and the mixture was stirred at 60° C. for 4 hours, filtered, and dried to obtain modified mica powder;

[0034] S2: Add 0.3 parts of chitosan to 50 parts of 3wt% acetic acid aqueous solution, add 0.15 parts of modified mica powder and stir evenly, add 3 parts of glutaraldehyde, stir at 60°C for 3 hours, filter, wash, and dry to obtain modified chitosan; add 2 parts of butyl betaine hydrochloride, 50 parts of water, 0.1 parts of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, and 0.2 parts of N-hydroxysuccinimide, stir at room temperature for 6 hours, filter, wash, and dry to obtain an antibacterial agent;

[0035] S3: 10 parts of antibacterial agent, 100 parts of water, and 2 parts of glutaraldehyde are mixed to obtain an antibacterial finishing liquid; the base composite cloth is mixed with the antibacterial finishing liquid in a mass ratio of 1:30, immersed at 60°C for 60 minutes, and rolled once, with a rolling rate of 88%, washed, and dried to obtain an antibacterial modified composite cloth;

[0036] S4: 10 parts of graphite were dispersed in 100 parts of a 50 wt% aqueous ethanol solution, ultrasonically dispersed for 3 hours, reacted at 160°C for 24 hours, washed, and dried to obtain porous graphene; the mixture was added to 40 parts of a mixed solution of concentrated sulfuric acid and phosphoric acid with a volume ratio of 9:1, stirred, and 0.03 parts of KMnO4 were slowly added, stirred at 60°C for 18 hours, the obtained suspension was poured into cold water, 30% H2O2 was added to terminate the reaction, washed, and dried to obtain hydroxylated porous graphene;

[0037] Take 0.3 parts of hydroxylated porous graphene, add 40 parts of dichloromethane and 5 parts of triethylamine under nitrogen atmosphere, stir evenly, ultrasonicate at room temperature for 3 hours, add 15 parts of acryloyl chloride dropwise over 1 hour, stir at 50°C for 24 hours, then add 15 parts of anhydrous ethanol, stir for 3 hours, wash, filter and dry to obtain double-bonded porous graphene;

[0038] S5: Take 4 parts of double-bonded porous graphene, 100 parts of water, 70 parts of ethanol, and 0.2 parts of BPO, mix them uniformly under ultrasonication, and under nitrogen protection, add 0.5 parts of double-bonded cooling agent, 0.1 parts of acrylic acid, 0.4 parts of 2-hydroxyethyl acrylate, 0.05-0.1 parts of 2-acrylamide-2-methylpropanesulfonic acid, and 0.1 parts of acrylamide, and react at 78°C with stirring for 12 hours. Wash, filter, and dry to obtain polymer-modified porous graphene;

[0039] S6: Add 18 parts of polymer-modified porous graphene to 100 parts of water, then add 2 parts of glutaraldehyde, and stir evenly to obtain a graphene finishing solution; mix the antibacterial modified composite cloth and the graphene finishing solution in a mass ratio of 1:30, immerse the cloth at 60°C for 90 minutes, perform one immersion and one rolling, and the rolling rate is 88%, bake the cloth at 160°C for 8 minutes, wash, and dry to obtain a cool composite denim cloth.

[0040] Example 2: S1: 40 parts of mica powder, 1 part of zinc oxide whisker, 80 parts of ethanol and 10 parts of water were mixed, the pH was adjusted to 4, 0.4 parts of KH550 were added, and the mixture was stirred at 60°C for 4 hours, filtered and dried to obtain modified mica powder;

[0041] S2: Add 0.3 parts of chitosan to 50 parts of 3wt% acetic acid aqueous solution, add 0.1 parts of modified mica powder and stir evenly, add 2 parts of glutaraldehyde, stir at 60°C for 3 hours, filter, wash, and dry to obtain modified chitosan; add 2 parts of butyl betaine hydrochloride, 50 parts of water, 0.1 parts of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, and 0.2 parts of N-hydroxysuccinimide, stir at room temperature for 6 hours, filter, wash, and dry to obtain an antibacterial agent;

[0042] S3: 10 parts of antibacterial agent, 100 parts of water, and 2 parts of glutaraldehyde are mixed to obtain an antibacterial finishing liquid; the base composite cloth is mixed with the antibacterial finishing liquid in a mass ratio of 1:30, immersed at 60°C for 60 minutes, and rolled once, with a rolling rate of 88%, washed, and dried to obtain an antibacterial modified composite cloth;

[0043] S4: 10 parts of graphite were dispersed in 100 parts of a 50 wt% aqueous ethanol solution, ultrasonically dispersed for 3 hours, reacted at 160°C for 24 hours, washed, and dried to obtain porous graphene; the mixture was added to 40 parts of a mixed solution of concentrated sulfuric acid and phosphoric acid with a volume ratio of 9:1, stirred, and 0.03 parts of KMnO4 were slowly added, stirred at 60°C for 18 hours, the obtained suspension was poured into cold water, 30% H2O2 was added to terminate the reaction, washed, and dried to obtain hydroxylated porous graphene;

[0044] Take 0.3 parts of hydroxylated porous graphene, add 40 parts of dichloromethane and 5 parts of triethylamine under nitrogen atmosphere, stir evenly, ultrasonicate at room temperature for 3 hours, add 15 parts of acryloyl chloride dropwise over 1 hour, stir at 50°C for 24 hours, then add 15 parts of anhydrous ethanol, stir for 3 hours, wash, filter and dry to obtain double-bonded porous graphene;

[0045] S5: 3 parts of double-bonded porous graphene, 100 parts of water, 70 parts of ethanol, and 0.2 parts of BPO were mixed by ultrasonication. Under nitrogen protection, 0.4 parts of double-bonded cooling agent, 0.2 parts of acrylic acid, 0.4 parts of 2-hydroxyethyl acrylate, 0.05 parts of 2-acrylamide-2-methylpropanesulfonic acid, and 0.1 parts of acrylamide were added. The mixture was stirred at 78°C for 12 hours, washed, filtered, and dried to obtain polymer-modified porous graphene.

[0046] S6: Add 18 parts of polymer-modified porous graphene to 100 parts of water, then add 2 parts of glutaraldehyde, and stir evenly to obtain a graphene finishing solution; mix the antibacterial modified composite cloth and the graphene finishing solution in a mass ratio of 1:30, immerse the cloth at 60°C for 90 minutes, perform one immersion and one rolling, and the rolling rate is 88%, bake the cloth at 160°C for 8 minutes, wash, and dry to obtain a cool composite denim cloth.

[0047] Comparative Example 1 (polymer-modified porous graphene was added with an antibacterial finishing liquid and the finishing was performed only once. The remaining steps were the same as those in Example 1): S1: 45 parts of mica powder and 2 parts of zinc oxide whiskers were mixed with 80 parts of ethanol and 10 parts of water, the pH was adjusted to 4, 0.5 parts of KH550 were added, and the mixture was stirred at 60° C. for 4 hours. The mixture was filtered and dried to obtain modified mica powder;

[0048] S2: Add 0.3 parts of chitosan to 50 parts of 3wt% acetic acid aqueous solution, add 0.15 parts of modified mica powder and stir evenly, add 3 parts of glutaraldehyde, stir at 60°C for 3 hours, filter, wash, and dry to obtain modified chitosan; add 2 parts of butyl betaine hydrochloride, 50 parts of water, 0.1 parts of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, and 0.2 parts of N-hydroxysuccinimide, stir at room temperature for 6 hours, filter, wash, and dry to obtain an antibacterial agent;

[0049] S3: 10 parts of graphite were dispersed in 100 parts of a 50 wt% aqueous ethanol solution, ultrasonically dispersed for 3 hours, reacted at 160°C for 24 hours, washed, and dried to obtain porous graphene; the mixture was added to 40 parts of a mixed solution of concentrated sulfuric acid and phosphoric acid in a volume ratio of 9:1, stirred, and 0.03 parts of KMnO4 were slowly added, stirred at 60°C for 18 hours, the obtained suspension was poured into cold water, 30% H2O2 was added to terminate the reaction, washed, and dried to obtain hydroxylated porous graphene;

[0050] Take 0.3 parts of hydroxylated porous graphene, add 40 parts of dichloromethane and 5 parts of triethylamine under nitrogen atmosphere, stir evenly, ultrasonicate at room temperature for 3 hours, add 15 parts of acryloyl chloride dropwise over 1 hour, stir at 50°C for 24 hours, then add 15 parts of anhydrous ethanol, stir for 3 hours, wash, filter and dry to obtain double-bonded porous graphene;

[0051] S4: 4 parts of double-bonded porous graphene, 100 parts of water, 70 parts of ethanol, and 0.2 parts of BPO were taken and ultrasonically mixed. Under nitrogen protection, 0.5 parts of double-bonded cooling agent, 0.1 parts of acrylic acid, 0.4 parts of 2-hydroxyethyl acrylate, 0.05-0.1 parts of 2-acrylamide-2-methylpropanesulfonic acid, and 0.1 parts of acrylamide were added. The mixture was stirred at 78°C for 12 hours, washed, filtered, and dried to obtain polymer-modified porous graphene.

[0052] S5: 10 parts of antibacterial agent, 18 parts of polymer-modified porous graphene, 100 parts of water, and 4 parts of glutaraldehyde are mixed to obtain an antibacterial finishing liquid: the base composite cloth and the antibacterial finishing liquid are mixed in a mass ratio of 1:30, immersed at 60°C for 60 minutes, and rolled once after dipping, with a rolling rate of 88%, baked at 160°C for 8 minutes, washed, and dried to obtain a cool composite denim.

[0053] Comparative Example 2 (graphite replaces porous graphene, and the method and steps are consistent with those in Example 1): S1: 45 parts of mica powder, 2 parts of zinc oxide whiskers, 80 parts of ethanol, and 10 parts of water are mixed, the pH is adjusted to 4, 0.5 parts of KH550 are added, and the mixture is stirred at 60° C. for 4 hours, filtered, and dried to obtain modified mica powder;

[0054] S2: Add 0.3 parts of chitosan to 50 parts of 3wt% acetic acid aqueous solution, add 0.15 parts of modified mica powder and stir evenly, add 3 parts of glutaraldehyde, stir at 60°C for 3 hours, filter, wash, and dry to obtain modified chitosan; add 2 parts of butyl betaine hydrochloride, 50 parts of water, 0.1 parts of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, and 0.2 parts of N-hydroxysuccinimide, stir at room temperature for 6 hours, filter, wash, and dry to obtain an antibacterial agent;

[0055] S3: 10 parts of antibacterial agent, 100 parts of water, and 2 parts of glutaraldehyde are mixed to obtain an antibacterial finishing liquid; the base composite cloth is mixed with the antibacterial finishing liquid in a mass ratio of 1:30, immersed at 60°C for 60 minutes, and rolled once, with a rolling rate of 88%, washed, and dried to obtain an antibacterial modified composite cloth;

[0056] S4: 10 parts of graphite were dispersed and added into 40 parts of a mixed solution of concentrated sulfuric acid and phosphoric acid in a volume ratio of 9:1, stirred and slowly added with 0.03 parts of KMnO4, stirred at 60°C for 18 hours, the obtained suspension was poured into cold water, 30% H2O2 was added to terminate the reaction, washed and dried to obtain hydroxylated porous graphene;

[0057] Take 0.3 parts of hydroxylated porous graphene, add 40 parts of dichloromethane and 5 parts of triethylamine under nitrogen atmosphere, stir evenly, ultrasonicate at room temperature for 3 hours, add 15 parts of acryloyl chloride dropwise over 1 hour, stir at 50°C for 24 hours, then add 15 parts of anhydrous ethanol, stir for 3 hours, wash, filter and dry to obtain double-bonded porous graphene;

[0058] S5: Take 4 parts of double-bonded porous graphene, 100 parts of water, 70 parts of ethanol, and 0.2 parts of BPO, mix them uniformly under ultrasonication, and under nitrogen protection, add 0.5 parts of double-bonded cooling agent, 0.1 parts of acrylic acid, 0.4 parts of 2-hydroxyethyl acrylate, 0.05-0.1 parts of 2-acrylamide-2-methylpropanesulfonic acid, and 0.1 parts of acrylamide, and react at 78°C with stirring for 12 hours. Wash, filter, and dry to obtain polymer-modified porous graphene;

[0059] S6: Add 18 parts of polymer-modified porous graphene to 100 parts of water, then add 2 parts of glutaraldehyde, and stir evenly to obtain a graphene finishing solution; mix the antibacterial modified composite cloth and the graphene finishing solution in a mass ratio of 1:30, immerse the cloth at 60°C for 90 minutes, perform one immersion and one rolling, and the rolling rate is 88%, bake the cloth at 160°C for 8 minutes, wash, and dry to obtain a cool composite denim cloth.

[0060] Comparative Example 3 (increasing the amount of polymer-modified porous graphene added, and the remaining method steps are consistent with Example 1): S1: After mixing 45 parts of mica powder, 2 parts of zinc oxide whiskers, 80 parts of ethanol, and 10 parts of water, the pH is adjusted to 4, 0.5 parts of KH550 are added, and the mixture is mixed and stirred at 60° C. for 4 hours, filtered, and dried to obtain modified mica powder;

[0061] S2: Add 0.3 parts of chitosan to 50 parts of 3wt% acetic acid aqueous solution, add 0.15 parts of modified mica powder and stir evenly, add 3 parts of glutaraldehyde, stir at 60°C for 3 hours, filter, wash, and dry to obtain modified chitosan; add 2 parts of butyl betaine hydrochloride, 50 parts of water, 0.1 parts of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, and 0.2 parts of N-hydroxysuccinimide, stir at room temperature for 6 hours, filter, wash, and dry to obtain an antibacterial agent;

[0062] S3: 10 parts of antibacterial agent, 100 parts of water, and 2 parts of glutaraldehyde are mixed to obtain an antibacterial finishing liquid; the base composite cloth is mixed with the antibacterial finishing liquid in a mass ratio of 1:30, immersed at 60°C for 60 minutes, and rolled once, with a rolling rate of 88%, washed, and dried to obtain an antibacterial modified composite cloth;

[0063] S4: 10 parts of graphite were dispersed in 100 parts of a 50 wt% aqueous ethanol solution, ultrasonically dispersed for 3 hours, reacted at 160°C for 24 hours, washed, and dried to obtain porous graphene; the mixture was added to 40 parts of a mixed solution of concentrated sulfuric acid and phosphoric acid with a volume ratio of 9:1, stirred, and 0.03 parts of KMnO4 were slowly added, stirred at 60°C for 18 hours, the obtained suspension was poured into cold water, 30% H2O2 was added to terminate the reaction, washed, and dried to obtain hydroxylated porous graphene;

[0064] Take 0.3 parts of hydroxylated porous graphene, add 40 parts of dichloromethane and 5 parts of triethylamine under nitrogen atmosphere, stir evenly, ultrasonicate at room temperature for 3 hours, add 15 parts of acryloyl chloride dropwise over 1 hour, stir at 50°C for 24 hours, then add 15 parts of anhydrous ethanol, stir for 3 hours, wash, filter and dry to obtain double-bonded porous graphene;

[0065] S5: Take 4 parts of double-bonded porous graphene, 100 parts of water, 70 parts of ethanol, and 0.2 parts of BPO, mix them uniformly under ultrasonication, and under nitrogen protection, add 0.5 parts of double-bonded cooling agent, 0.1 parts of acrylic acid, 0.4 parts of 2-hydroxyethyl acrylate, 0.05-0.1 parts of 2-acrylamide-2-methylpropanesulfonic acid, and 0.1 parts of acrylamide, and react at 78°C with stirring for 12 hours. Wash, filter, and dry to obtain polymer-modified porous graphene;

[0066] S6: Add 25 parts of polymer-modified porous graphene to 100 parts of water, then add 2 parts of glutaraldehyde, and stir evenly to obtain a graphene finishing solution; mix the antibacterial modified composite cloth and the graphene finishing solution in a mass ratio of 1:30, immerse the cloth at 60°C for 90 minutes, perform one immersion and one rolling, and the rolling rate is 88%, bake the cloth at 160°C for 8 minutes, wash, and dry to obtain a cool composite denim cloth.

[0067] Comparative Example 4 (the formula of the graphene finishing liquid was changed, and the remaining method steps were consistent with Example 1): S1: 45 parts of mica powder, 2 parts of zinc oxide whiskers, 80 parts of ethanol, and 10 parts of water were mixed, the pH was adjusted to 4, 0.5 parts of KH550 were added, and the mixture was mixed and stirred at 60° C. for 4 hours, filtered, and dried to obtain modified mica powder;

[0068] S2: Add 0.3 parts of chitosan to 50 parts of 3wt% acetic acid aqueous solution, add 0.15 parts of modified mica powder and stir evenly, add 3 parts of glutaraldehyde, stir at 60°C for 3 hours, filter, wash, and dry to obtain modified chitosan; add 2 parts of butyl betaine hydrochloride, 50 parts of water, 0.1 parts of 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide, and 0.2 parts of N-hydroxysuccinimide, stir at room temperature for 6 hours, filter, wash, and dry to obtain an antibacterial agent;

[0069] S3: 10 parts of antibacterial agent, 100 parts of water, and 2 parts of glutaraldehyde are mixed to obtain an antibacterial finishing liquid; the base composite cloth is mixed with the antibacterial finishing liquid in a mass ratio of 1:30, immersed at 60°C for 60 minutes, and rolled once, with a rolling rate of 88%, washed, and dried to obtain an antibacterial modified composite cloth;

[0070] S4: 10 parts of graphite were dispersed in 100 parts of a 50 wt% aqueous ethanol solution, ultrasonically dispersed for 3 hours, reacted at 160°C for 24 hours, washed, and dried to obtain porous graphene; the mixture was added to 40 parts of a mixed solution of concentrated sulfuric acid and phosphoric acid with a volume ratio of 9:1, stirred, and 0.03 parts of KMnO4 were slowly added, stirred at 60°C for 18 hours, the obtained suspension was poured into cold water, 30% H2O2 was added to terminate the reaction, washed, and dried to obtain hydroxylated porous graphene;

[0071] Take 0.3 parts of hydroxylated porous graphene, add 40 parts of dichloromethane and 5 parts of triethylamine under nitrogen atmosphere, stir evenly, ultrasonicate at room temperature for 3 hours, add 15 parts of acryloyl chloride dropwise over 1 hour, stir at 50°C for 24 hours, then add 15 parts of anhydrous ethanol, stir for 3 hours, wash, filter and dry to obtain double-bonded porous graphene;

[0072] S5: Add 16 parts of double-bonded porous graphene and 2 parts of double-bonded cooling agent to 100 parts of water, then add 0.02 parts of BPO, and stir evenly to obtain a graphene finishing liquid; mix the antibacterial modified composite cloth and the graphene finishing liquid in a mass ratio of 1:30, immerse the cloth at 80°C for 120 minutes, perform one immersion and one rolling, and the rolling rate is 88%, bake the cloth at 160°C for 8 minutes, wash, and dry to obtain a cool composite denim cloth.

[0073] Performance test: (1) Take the cool composite denim prepared in Examples 1 to 2 and Comparative Examples 1 to 4; (2) With reference to GB / T20944.3-2008, select Escherichia coli and measure the antibacterial property and the antibacterial property after washing 50 times; (3) With reference to GB / T5453, measure the air permeability; see Table 1 for details;

[0074] Table 1:

[0075]

[0076] Conclusion: In comparative example 1, polymer-modified porous graphene was added to the antibacterial finishing liquid, and only one finishing was performed, and the performance decreased, which may be due to the adverse effects caused by the mutual influence of the two finishing agents; in comparative example 2, graphite was used instead of porous graphene, and the performance was obviously inferior to that of the embodiment; in comparative example 3, the amount of polymer-modified porous graphene added was increased, which affected the air permeability, from which it can be seen that the amount added needs to be controlled; in comparative example 4, the formula of the graphene finishing liquid was changed, and double-bonded porous graphene, double-bonded cooling agent, and BPO were added to water to obtain the graphene finishing liquid, and the performance decreased, which may be due to the decrease in dispersibility; in summary, the cool composite denim prepared by the present invention has good wash resistance while maintaining good antibacterial and breathable properties.

[0077] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art will be able to modify the technical solutions described in the aforementioned embodiments or substitute equivalents for some of the technical features. Any modifications, equivalent substitutions, and improvements made within the spirit and principles of the present invention shall be included within the scope of protection of the present invention.

Claims

1. A method for preparing a cool composite denim fabric containing mint fiber, characterized by: The following steps are involved: S1: inner layer fabric made of mint nylon filament; S2: Using cotton-viscose blended siro-spun 21-count yarn as the warp yarn and natural mint fiber and cotton blended stretch yarn as the weft yarn, a mint fiber-containing denim fabric was prepared as the surface fabric; the warp yarns were interwoven with the weft yarns in a three-up, one-down right twill. S3: Laminating the inner layer fabric and the outer layer fabric, stacking and aligning them, and sewing them to obtain the basic composite fabric; S4: treating the base composite fabric with an antibacterial finishing liquid to obtain an antibacterial modified composite fabric; S5: The antibacterial modified composite fabric is treated with a graphene finishing liquid to obtain a cool composite denim fabric.

2. The method for preparing a cool composite denim fabric containing mint fiber according to claim 1, characterized in that: The antibacterial finishing liquid comprises the following raw materials, calculated by weight: 10 to 12 parts of antibacterial agent, 100 parts of water, and 2 to 3 parts of glutaraldehyde; The preparation of the antibacterial agent comprises the following steps: mixing mica powder, zinc oxide whiskers, ethanol and water, adjusting the pH to 3-5, adding a coupling agent, stirring at 50-70° C. for 2-4 hours, filtering and drying to obtain modified mica powder; Add chitosan to acetic acid aqueous solution, add modified mica powder and stir evenly, add glutaraldehyde, stir and react at 50-60°C for 2-3 hours, filter, wash and dry to obtain modified chitosan; add butyl betaine hydrochloride, water, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide and N-hydroxysuccinimide, stir for 5-6 hours, filter, wash and dry to obtain an antibacterial agent.

3. The method for preparing a cool composite denim containing mint fiber according to claim 2, characterized in that: The modified mica powder comprises the following raw materials, calculated by mass: 40 to 50 parts of mica powder, 1 to 2 parts of zinc oxide whiskers, 60 to 80 parts of ethanol, 10 to 15 parts of water, and 0.2 to 0.6 parts of a coupling agent; The antibacterial agent comprises the following raw materials, calculated by weight: 0.3-0.5 parts of chitosan, 0.1-0.2 parts of modified mica powder, 2-4 parts of glutaraldehyde, and 2-3 parts of butyl betaine hydrochloride.

4. The method for preparing a cool composite denim containing mint fiber according to claim 1, characterized in that: The specific steps of S4 are: mixing the base composite cloth and the antibacterial finishing liquid in a mass ratio of 1:30-50, dipping at a temperature of 50-60°C for 60-100 minutes, dipping and rolling, with a rolling rate of 80-90%, washing and drying to obtain the antibacterial modified composite cloth.

5. The method for preparing a cool composite denim containing mint fiber according to claim 1, characterized in that: The graphene finishing solution includes the following raw materials, calculated by weight: 15 to 20 parts of polymer-modified porous graphene, 100 parts of water, and 1 to 2 parts of glutaraldehyde; The preparation of polymer-modified porous graphene includes the following steps: taking cinnamoyl chloride, pyridine, and menthol, stirring at 40-50° C. for 4-5 hours, and post-processing and purification to obtain a double-bonded cooling agent; taking double-bonded porous graphene, water, ethanol, and an initiator, ultrasonically mixing them uniformly, adding the double-bonded cooling agent, acrylic acid, 2-hydroxyethyl acrylic acid, 2-acrylamide-2-methylpropanesulfonic acid, and acrylamide under nitrogen protection, stirring and reacting at 75-78° C. for 8-12 hours, washing, filtering, and drying to obtain polymer-modified porous graphene.

6. The method for preparing a cool composite denim fabric containing mint fiber according to claim 5, characterized in that: The double-bonded cooling agent includes the following raw materials, calculated in parts by mass: 1 to 2 parts of cinnamoyl chloride, 5 to 6 parts of pyridine, and 1 to 2 parts of menthol; the polymer-modified porous graphene includes the following raw materials, calculated in parts by mass: 3 to 5 parts of double-bonded porous graphene, 0.1 to 0.3 parts of initiator, 0.4 to 0.6 parts of double-bonded cooling agent, 0.1 to 0.2 parts of acrylic acid, 0.3 to 0.4 parts of 2-hydroxyethyl acrylate, 0.05 to 0.1 parts of 2-acrylamide-2-methylpropanesulfonic acid, and 0.1 to 0.2 parts of acrylamide.

7. The method for preparing a cool composite denim fabric containing mint fiber according to claim 1, characterized in that: The specific steps of S5 are: mixing the antibacterial modified composite cloth and the graphene finishing liquid in a mass ratio of 1:30-50, dipping at a temperature of 50-60°C for 60-100 minutes, dipping and rolling once, with a rolling rate of 80-90%, baking at a temperature of 150-170°C for 5-10 minutes, washing, and drying to obtain a cool composite denim cloth.

8. The cool composite denim fabric prepared according to the method for preparing a cool composite denim fabric containing mint fiber according to any one of claims 1 to 7.

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