Antibacterial moisture-absorption breathable pure cotton fabric, preparation method and application in non-sensitization underwear
By grafting nano zinc oxide and betaine on cotton fibers and combining them with antibacterial finishing reactions, the problem of insufficient antibacterial properties of pure cotton fabrics was solved, and efficient antibacterial, moisture absorption and breathable effects were achieved.
Patent Information
- Application Number
- CN202510805255.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-17
- Publication Date
- 2025-09-23
- Estimated Expiration
- 2045-06-17
AI Technical Summary
The antibacterial properties of existing pure cotton fabrics need to be improved, as they are prone to breeding microorganisms and causing skin allergic reactions.
By grafting modification treatment on cotton fibers, the inorganic antibacterial component nano zinc oxide and the organic antibacterial component betaine are introduced, and an air layer is formed through the knitting process, combined with the antibacterial finishing reaction to improve the antibacterial performance.
It significantly improves the antibacterial properties of cotton fibers, reduces skin irritation, and improves moisture absorption, breathability and warmth retention.
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Figure CN120680765A_ABST
Abstract
Description
Technical Field
[0001] The present invention belongs to the technical field of fabrics, and in particular relates to an antibacterial, moisture-absorbing, breathable pure cotton fabric, a preparation method, and application in non-allergenic underwear. Background Art
[0002] Pure cotton fabrics are made from natural plant fibers, offering excellent warmth retention, a soft feel, excellent moisture absorption, and breathability, reducing skin irritation and preventing allergies. However, when worn, bodily secretions like sweat and sebum adhere to cotton fabrics, creating a favorable habitat for harmful microorganisms, promoting their growth and reproduction, and potentially causing health issues such as skin allergies. Therefore, antimicrobial modification of pure cotton fabrics is necessary to enhance their protective properties.
[0003] Chinese patent CN104264464B discloses a method for preparing organic cationic-modified textile fibers. Using cotton fiber as a carrier, a quaternization reaction between an organic cationic precursor and epichlorohydrin forms an organic cationic compound containing active epoxy or dihydroxy groups. Quaternary ammonium salts and quaternary phosphonium salts are then grafted onto the surface of the cotton fiber to create a cotton textile material with durable antimicrobial properties. However, the molecular structure of cotton fiber is stable, and the number of active groups capable of grafting with epoxy groups is limited, leaving room for improvement in antimicrobial properties. Summary of the Invention
[0004] In view of the deficiencies in the prior art, the present invention provides an antibacterial, moisture-absorbing and breathable pure cotton fabric to solve the problem in the prior art that the antibacterial performance of pure cotton fabrics needs to be improved.
[0005] In order to achieve the above object, the technical solution adopted by the present invention is as follows: a method for preparing an antibacterial, moisture-absorbing and breathable pure cotton fabric comprises the following steps: Step 1: dissolving dimethylaminoethyl methacrylate in methanol, adding chlorinated modified nano zinc oxide and potassium iodide, reacting, filtering, washing, and drying after the reaction is completed to obtain olefin-modified nano zinc oxide; Step 2: adding cotton fiber, cerium ammonium nitrate, olefin-modified nano zinc oxide, methacryloylethyl sulfobetaine, and a buffer to a nitric acid aqueous solution for reaction. After the reaction is completed, the cotton fiber is removed, washed, and dried to obtain grafted cotton fiber; the buffer is selected from one or a combination of acetic acid and sodium acetate, citric acid and sodium citrate, and is used to adjust the pH of the nitric acid aqueous solution to 4.0-5.5; Step 3: first spinning the grafted cotton fiber into pure cotton yarn, and then spinning the pure cotton yarn into pure cotton fabric through a knitting process; Step 4: soaking the pure cotton fabric in a polyhexamethyleneguanidine hydrochloride aqueous solution for reaction. After the reaction is completed, taking out, washing, and drying to obtain a modified pure cotton fabric; Step 5: Use the modified pure cotton fabric as the outer fabric and the inner fabric respectively, and compound the outer fabric and the inner fabric with equal areas to obtain an antibacterial, moisture-absorbing and breathable pure cotton fabric.
[0006] Preferably, in step 1, the mass ratio of dimethylaminoethyl methacrylate, chloride-modified nano-zinc oxide, potassium iodide, and methanol is 15.7:(8.9-9.3):(0.85-0.9):(60-80), and the reaction conditions are reflux reaction at 65-75°C under nitrogen protection for 10-20 hours.
[0007] Preferably, the chlorination-modified nano zinc oxide is prepared by the following steps: adding nano zinc oxide to ethanol, ultrasonicating, adding 3-chloropropyltrimethoxysilane, reacting, adjusting the pH value to 4-5 after the reaction, continuing the reaction, filtering, washing, and drying to obtain chlorination-modified nano zinc oxide.
[0008] Preferably, the mass ratio of nano zinc oxide, ethanol, and 3-chloropropyltrimethoxysilane is 8.1:(250-300):(20-25), and the reaction conditions are 80-90° C. for 20-40 minutes, and the continued reaction conditions are 80-90° C. for 3-4 hours.
[0009] Preferably, in the step 2, the mass ratio of cotton fiber, cerium ammonium nitrate, alkenyl-modified nano zinc oxide, methacryloylethyl sulfobetaine, buffer and nitric acid aqueous solution is 10:(0.7–0.9):(2–4):(3–6):(0.5–2):(100–150), and the reaction conditions are under nitrogen protection and at a temperature of 25-35° C. for 2.5-3.5 hours; the buffer is selected from one or a combination of acetic acid and sodium acetate, citric acid and sodium citrate, and is used to adjust the pH of the nitric acid aqueous solution to 4.0–5.5; the concentration of nitric acid in the nitric acid aqueous solution is 0.08-0.12 mol / L.
[0010] Preferably, in step 3, the yarn count of the pure cotton yarn is 30-50S (English count), and the weight of the pure cotton fabric is 180-220g / m 2 .
[0011] Preferably, in the step 4, the bath ratio of the pure cotton fabric to the polyhexamethyleneguanidine hydrochloride aqueous solution is 1:(45-55), and the reaction conditions are 50-60° C. for 2-3 hours; the concentration of polyhexamethyleneguanidine hydrochloride in the polyhexamethyleneguanidine hydrochloride aqueous solution is 4-6 g / L.
[0012] The present invention also discloses an antibacterial, moisture-absorbing, breathable pure cotton fabric prepared by adopting the above-mentioned method for preparing the antibacterial, moisture-absorbing, breathable pure cotton fabric.
[0013] The invention discloses an application of the above-mentioned antibacterial, moisture-absorbing and breathable pure cotton fabric in non-allergenic underwear.
[0014] Compared with the prior art, the present invention has the following beneficial effects: the present invention uses cotton fiber to prepare fabric, which has good moisture absorption and air permeability; the fabric includes an inner layer fabric and an outer layer fabric, and an air layer is formed by the gap between the two layers of fabric, which can improve the thermal insulation performance of the fabric; the cotton fiber is subjected to grafting modification treatment, and an inorganic antibacterial component nano zinc oxide and an organic antibacterial component betaine are introduced, which can effectively improve the antibacterial performance of the cotton fiber; the pure cotton fabric spun from the grafted cotton fiber can further improve the antibacterial performance after antibacterial finishing; in the present invention, when preparing the grafted cotton fiber, dimethylaminoethyl methacrylate and chlorinated modified nano zinc oxide react under the action of potassium iodide catalyst to obtain olefin-modified nano zinc oxide, and while forming an antibacterial quaternary ammonium salt on the surface of the nano zinc oxide, a carbon-carbon double bond (-C=C-) is introduced; under the action of a Ce(IV) salt initiator, under acidic conditions, a free radical is formed between the C2-C3 bond of the cotton fiber molecular skeleton through a single electron transfer process, and then reacts with the carbon atoms on the olefin-modified nano zinc oxide and the methacryloylethyl sulfobetaine molecule. The carbon double bond undergoes a graft copolymerization reaction, and the inorganic antibacterial component nano zinc oxide and the organic antibacterial component betaine are grafted onto the cotton fiber molecules, which can not only effectively improve the antibacterial properties of the cotton fiber, but the introduced betaine also has an anti-allergic effect, can reduce skin irritation and prevent sensitization; in the present invention, when the grafted cotton fiber is prepared under the action of an initiator, free radicals are formed between the C2-C3 bonds of the cotton fiber molecular skeleton, and aldehyde groups are formed at the same time. The pure cotton fabric is immersed in a polyhexamethyleneguanidine hydrochloride aqueous solution for antibacterial finishing reaction, and the aldehyde groups can react with The amino groups at the end of polyhexamethyleneguanidine hydrochloride react to introduce antibacterial guanidine salts into the cotton fiber fabric through chemical bonding, forming an antibacterial Schiff base structure (-C=N-), which can further enhance the antibacterial performance. In addition, the antibacterial components quaternary ammonium salts, betaine and guanidine salts all have excellent hydrophilicity, which can further enhance the moisture absorption and breathability of pure cotton fabrics. Pure cotton fabrics are spun through a knitting process, and there are many tiny pores between the yarns, allowing air to circulate freely, thereby further enhancing the breathability of pure cotton fabrics. BRIEF DESCRIPTION OF THE DRAWINGS
[0015] Figure 1 This is a flow chart of the preparation process of the modified pure cotton fabric of the present invention; Figure 2 This is a bar graph showing the test results of moisture permeability of the antibacterial, moisture-absorbing, breathable pure cotton fabrics prepared in Examples 1-5 of the present invention and Comparative Examples 1-3; Figure 3 This is a bar graph showing the air permeability test results of the antibacterial, moisture-absorbing, breathable pure cotton fabrics prepared in Examples 1-5 of the present invention and Comparative Examples 1-3; Figure 4 This is a bar chart showing the antibacterial performance test results of the antibacterial, moisture-absorbing, and breathable pure cotton fabrics prepared in Examples 1-5 of the present invention and Comparative Examples 1-3. DETAILED DESCRIPTION
[0016] Example 1 This embodiment discloses a method for preparing an antibacterial, moisture-absorbing, breathable pure cotton fabric, comprising the following steps: Step 1: dissolving dimethylaminoethyl methacrylate in methanol, adding chlorinated modified nano zinc oxide and potassium iodide, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, and methanol is 15.7:8.9:0.85:60, and reflux reaction at 65°C for 30 hours under nitrogen protection. After the reaction is completed, filtering, washing with ethanol 3 times, and placing in a vacuum drying oven at 60°C to dry to constant weight to obtain olefin-modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: : Add nano zinc oxide to ethanol, ultrasonicate at 50 kHz for 30 minutes, then add 3-chloropropyltrimethoxysilane, the mass ratio of nano zinc oxide, ethanol, and 3-chloropropyltrimethoxysilane is 8.1:250:20, react at 80°C for 40 minutes, add 2 mol / L hydrochloric acid aqueous solution to adjust the pH to 4, and continue to react at 80°C for 4 hours. After the reaction is completed, filter, wash with ethanol three times, and dry in a vacuum drying oven at 60°C to constant weight to obtain chloride-modified nano zinc oxide; Step 2, adding cotton fiber, ceric ammonium nitrate, alkenyl-modified nano zinc oxide, methacryloylethyl sulfonyl betaine and a buffer to a 0.08 mol / L nitric acid aqueous solution, wherein the mass ratio of cotton fiber, ceric ammonium nitrate, alkenyl-modified nano zinc oxide, methacryloylethyl sulfonyl betaine, buffer and 0.08 mol / L nitric acid aqueous solution is 10:0.7:2:3:1:100; the buffer is selected as a combination of acetic acid and sodium acetate in a ratio of 1:1, which is used to adjust the pH of the nitric acid aqueous solution to 5.0; under nitrogen protection, the reaction is carried out at a temperature of 25°C for 3.5 hours. After the reaction is completed, the cotton fiber is taken out and thoroughly washed with deionized water to remove the initiator ceric ammonium nitrate, nitric acid, unreacted alkenyl-modified nano zinc oxide and methacryloylethyl sulfonyl betaine on the surface of the cotton fiber to obtain a grafted cotton fiber; Step 3: First, the grafted cotton fiber is spun into pure cotton yarn with a yarn count of 40S. Then, the pure cotton yarn is spun into pure cotton fabric through a knitting process. The weight of the pure cotton fabric is 200g / m 2 ; Step 4: Immerse the pure cotton fabric in a 4 g / L polyhexamethyleneguanidine hydrochloride aqueous solution at a bath ratio of 1:55, react at 50° C. for 3 h, and after the reaction is completed, take out the fabric, wash it with deionized water 5 times, and dry it at room temperature to obtain a modified pure cotton fabric; Step 5: Use the modified pure cotton fabric as the outer fabric and the inner fabric respectively, and use cotton thread to sew the outer fabric and the inner fabric of equal area to obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.
[0017] Example 2 This embodiment discloses a method for preparing an antibacterial, moisture-absorbing, breathable pure cotton fabric, comprising the following steps: Step 1: dissolving dimethylaminoethyl methacrylate in methanol, adding chlorinated nano zinc oxide and potassium iodide, the mass ratio of dimethylaminoethyl methacrylate, chlorinated nano zinc oxide, potassium iodide, and methanol is 15.7:9.3:0.9:80, and reflux reaction is carried out at 75°C under nitrogen protection for 20 hours. After the reaction is completed, filtering, washing with ethanol three times, and placing in a vacuum drying oven at 60°C to constant weight to obtain olefin-modified nano zinc oxide; wherein, the chlorinated nano zinc oxide is prepared by the following steps: Nano-zinc oxide was added to ethanol, and after ultrasonication at a frequency of 50 kHz for 30 minutes, 3-chloropropyltrimethoxysilane was added, and the mass ratio of nano-zinc oxide, ethanol, and 3-chloropropyltrimethoxysilane was 8.1:300:25. After reacting at a temperature of 90°C for 20 minutes, a 2 mol / L aqueous hydrochloric acid solution was added to adjust the pH value to 5, and the reaction was continued at a temperature of 90°C for 3 hours. After the reaction was completed, the mixture was filtered, washed with ethanol three times, and dried in a vacuum drying oven at 60°C to constant weight to obtain chlorinated modified nano-zinc oxide; Step 2, adding cotton fiber, ceric ammonium nitrate, alkenyl-modified nano zinc oxide, and methacryloylethyl sulfonyl betaine to a 0.12 mol / L nitric acid aqueous solution, wherein the mass ratio of cotton fiber, ceric ammonium nitrate, alkenyl-modified nano zinc oxide, methacryloylethyl sulfonyl betaine, and 0.12 mol / L nitric acid aqueous solution is 10:0.9:4:6:150, reacting at 35°C under nitrogen protection for 2.5 hours. After the reaction is completed, taking out the cotton fiber, washing it thoroughly with deionized water to remove the initiator ceric ammonium nitrate, nitric acid, unreacted alkenyl-modified nano zinc oxide, and methacryloylethyl sulfonyl betaine on the surface of the cotton fiber, and obtaining a grafted cotton fiber; Step 3: First, the grafted cotton fiber is spun into pure cotton yarn with a yarn count of 40S. Then, the pure cotton yarn is spun into pure cotton fabric through a knitting process. The weight of the pure cotton fabric is 200g / m 2 ; Step 4: immersing the pure cotton fabric in a 6 g / L polyhexamethyleneguanidine hydrochloride aqueous solution at a bath ratio of 1:45, reacting the fabric at 60° C. for 2 h. After the reaction is complete, taking the fabric out, washing it with deionized water 5 times, and drying it at room temperature to obtain a modified pure cotton fabric; Step 5: Use the modified pure cotton fabric as the outer fabric and the inner fabric respectively, and use cotton thread to sew the outer fabric and the inner fabric of equal area to obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.
[0018] Example 3 This embodiment discloses a method for preparing an antibacterial, moisture-absorbing, breathable pure cotton fabric, comprising the following steps: Step 1: dissolve dimethylaminoethyl methacrylate in methanol, add chlorinated modified nano zinc oxide and potassium iodide, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, and methanol is 15.7:9:0.86:65, and reflux at 70°C for 24 hours under nitrogen protection. After the reaction is completed, filter, wash with ethanol 3 times, and place in a vacuum drying oven at 60°C to dry to constant weight to obtain olefin-modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: dissolving nano zinc oxide; chlorinated modified ... Nano zinc oxide was added to ethanol, and after ultrasonication at a frequency of 50 kHz for 30 minutes, 3-chloropropyltrimethoxysilane was added. The mass ratio of nano zinc oxide, ethanol, and 3-chloropropyltrimethoxysilane was 8.1:260:21. After reacting at 85°C for 30 minutes, a 2 mol / L aqueous hydrochloric acid solution was added to adjust the pH value to 4.5. The reaction was continued at 85°C for 3.5 hours. After the reaction was completed, the mixture was filtered, washed with ethanol three times, and dried in a vacuum drying oven at 60°C to constant weight to obtain chloride-modified nano zinc oxide. Step 2, adding cotton fiber, ceric ammonium nitrate, alkenyl-modified nano zinc oxide, and methacryloylethyl sulfonyl betaine to a 0.09 mol / L nitric acid aqueous solution, wherein the mass ratio of cotton fiber, ceric ammonium nitrate, alkenyl-modified nano zinc oxide, methacryloylethyl sulfonyl betaine, and 0.09 mol / L nitric acid aqueous solution is 10:0.75:2.5:4:110, and reacting at 30°C under nitrogen protection for 3 hours. After the reaction is completed, taking out the cotton fiber, and washing it thoroughly with deionized water to remove the initiator ceric ammonium nitrate, nitric acid, and unreacted alkenyl-modified nano zinc oxide and methacryloylethyl sulfonyl betaine on the surface of the cotton fiber to obtain a grafted cotton fiber; Step 3: First, the grafted cotton fiber is spun into pure cotton yarn with a yarn count of 40S. Then, the pure cotton yarn is spun into pure cotton fabric through a knitting process. The weight of the pure cotton fabric is 200g / m 2 ; Step 4: Immerse the pure cotton fabric in a 4.5 g / L polyhexamethyleneguanidine hydrochloride aqueous solution at a bath ratio of 1:50, react at 55° C. for 2.5 h, and after the reaction is completed, take out the fabric, wash it with deionized water 5 times, and dry it at room temperature to obtain a modified pure cotton fabric; Step 5: Use the modified pure cotton fabric as the outer fabric and the inner fabric respectively, and use cotton thread to sew the outer fabric and the inner fabric of equal area to obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.
[0019] Example 4 This embodiment discloses a method for preparing an antibacterial, moisture-absorbing, breathable pure cotton fabric, comprising the following steps: Step 1: dissolve dimethylaminoethyl methacrylate in methanol, add chlorinated modified nano zinc oxide and potassium iodide, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, and methanol is 15.7:9.1:0.87:70, and reflux at 70°C for 24 hours under nitrogen protection. After the reaction is completed, filter, wash with ethanol 3 times, and place in a vacuum drying oven at 60°C to dry to constant weight to obtain olefin-modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: dissolving nano zinc oxide; chlorinated modified ... Nano zinc oxide was added to ethanol, and after ultrasonication at a frequency of 50 kHz for 30 minutes, 3-chloropropyltrimethoxysilane was added. The mass ratio of nano zinc oxide, ethanol, and 3-chloropropyltrimethoxysilane was 8.1:275:22.5. After the reaction was carried out at 85°C for 30 minutes, a 2 mol / L aqueous hydrochloric acid solution was added to adjust the pH value to 4.5. The reaction was continued at 85°C for 3.5 hours. After the reaction was completed, the mixture was filtered, washed with ethanol three times, and dried in a vacuum drying oven at 60°C to constant weight to obtain chloride-modified nano zinc oxide. Step 2, adding cotton fiber, ceric ammonium nitrate, alkenyl-modified nano zinc oxide, and methacryloylethyl sulfonyl betaine to a 0.1 mol / L nitric acid aqueous solution, wherein the mass ratio of cotton fiber, ceric ammonium nitrate, alkenyl-modified nano zinc oxide, methacryloylethyl sulfonyl betaine, and 0.1 mol / L nitric acid aqueous solution is 10:0.8:3:4.5:125, and reacting at 30°C under nitrogen protection for 3 hours. After the reaction is completed, taking out the cotton fiber, and washing it thoroughly with deionized water to remove the initiator ceric ammonium nitrate, nitric acid, and unreacted alkenyl-modified nano zinc oxide and methacryloylethyl sulfonyl betaine on the surface of the cotton fiber to obtain a grafted cotton fiber; Step 3: First, the grafted cotton fiber is spun into pure cotton yarn with a yarn count of 40S. Then, the pure cotton yarn is spun into pure cotton fabric through a knitting process. The weight of the pure cotton fabric is 200g / m 2 ; Step 4: Immerse the pure cotton fabric in a 5 g / L polyhexamethyleneguanidine hydrochloride aqueous solution at a bath ratio of 1:50, react at 55° C. for 2.5 h, and after the reaction is completed, take out the fabric, wash it with deionized water 5 times, and dry it at room temperature to obtain a modified pure cotton fabric; Step 5: Use the modified pure cotton fabric as the outer fabric and the inner fabric respectively, and use cotton thread to sew the outer fabric and the inner fabric of equal area to obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.
[0020] Example 5 This embodiment discloses a method for preparing an antibacterial, moisture-absorbing, breathable pure cotton fabric, comprising the following steps: Step 1: dissolve dimethylaminoethyl methacrylate in methanol, add chlorinated modified nano zinc oxide and potassium iodide, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, and methanol is 15.7:9.2:0.88:75, and reflux at 70°C for 24 hours under nitrogen protection. After the reaction is completed, filter, wash with ethanol three times, and place in a vacuum drying oven at 60°C to dry to constant weight to obtain olefin-modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: Nano-zinc oxide was added to ethanol, and after ultrasonication at a frequency of 50 kHz for 30 minutes, 3-chloropropyltrimethoxysilane was added, and the mass ratio of nano-zinc oxide, ethanol, and 3-chloropropyltrimethoxysilane was 8.1:290:24. After the reaction was carried out at 85°C for 30 minutes, a 2 mol / L aqueous hydrochloric acid solution was added to adjust the pH value to 4.5. The reaction was continued at 85°C for 3.5 hours. After the reaction was completed, the mixture was filtered, washed with ethanol three times, and dried in a vacuum drying oven at 60°C to constant weight to obtain chloride-modified nano-zinc oxide; Step 2, adding cotton fiber, ammonium cerium nitrate, alkenyl-modified nano zinc oxide, and methacryloylethyl sulfonyl betaine to a 0.11 mol / L nitric acid aqueous solution, wherein the mass ratio of cotton fiber, ammonium cerium nitrate, alkenyl-modified nano zinc oxide, methacryloylethyl sulfonyl betaine, and 0.11 mol / L nitric acid aqueous solution is 10:0.85:3.5:5:140, and reacting at 30°C under nitrogen protection for 3 hours. After the reaction is completed, taking out the cotton fiber, and washing it thoroughly with deionized water to remove the initiator ammonium cerium nitrate, nitric acid, and unreacted alkenyl-modified nano zinc oxide and methacryloylethyl sulfonyl betaine on the surface of the cotton fiber to obtain a grafted cotton fiber; Step 3: First, the grafted cotton fiber is spun into pure cotton yarn with a yarn count of 40S. Then, the pure cotton yarn is spun into pure cotton fabric through a knitting process. The weight of the pure cotton fabric is 200g / m 2 ; Step 4: Immerse the pure cotton fabric in a 5.5 g / L polyhexamethyleneguanidine hydrochloride aqueous solution at a bath ratio of 1:50, react at 55° C. for 2.5 h, and after the reaction is completed, take out the fabric, wash it with deionized water 5 times, and dry it at room temperature to obtain a modified pure cotton fabric; Step 5: Use the modified pure cotton fabric as the outer fabric and the inner fabric respectively, and use cotton thread to sew the outer fabric and the inner fabric of equal area to obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.
[0021] Comparative Example 1 This comparative example discloses a method for preparing an antibacterial, moisture-absorbing, breathable pure cotton fabric, comprising the following steps: Step 1: dissolving dimethylaminoethyl methacrylate in methanol, adding chlorinated modified nano zinc oxide and potassium iodide, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, and methanol is 15.7:8.9:0.85:60, and reflux reaction at 65°C for 30 hours under nitrogen protection. After the reaction is completed, filtering, washing with ethanol 3 times, and placing in a vacuum drying oven at 60°C to dry to constant weight to obtain olefin-modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: : Add nano zinc oxide to ethanol, ultrasonicate at 50 kHz for 30 minutes, then add 3-chloropropyltrimethoxysilane, the mass ratio of nano zinc oxide, ethanol, and 3-chloropropyltrimethoxysilane is 8.1:250:20, react at 80°C for 40 minutes, add 2 mol / L hydrochloric acid aqueous solution to adjust the pH to 4, and continue to react at 80°C for 4 hours. After the reaction is completed, filter, wash with ethanol three times, and dry in a vacuum drying oven at 60°C to constant weight to obtain chloride-modified nano zinc oxide; Step 2, adding cotton fiber, ammonium cerium nitrate, and alkenyl-modified nano-zinc oxide to a 0.08 mol / L nitric acid aqueous solution, wherein the mass ratio of cotton fiber, ammonium cerium nitrate, alkenyl-modified nano-zinc oxide, and 0.08 mol / L nitric acid aqueous solution is 10:0.7:2:100, and reacting at 25°C under nitrogen protection for 3.5 hours. After the reaction is completed, taking out the cotton fiber, and washing it thoroughly with deionized water to remove the initiator ammonium cerium nitrate, nitric acid, unreacted alkenyl-modified nano-zinc oxide, and methacryloylethyl sulfobetaine on the surface of the cotton fiber to obtain a grafted cotton fiber; Step 3: First, the grafted cotton fiber is spun into pure cotton yarn with a yarn count of 40S. Then, the pure cotton yarn is spun into pure cotton fabric through a knitting process. The weight of the pure cotton fabric is 200g / m 2 ; Step 4: Immerse the pure cotton fabric in a 4 g / L polyhexamethyleneguanidine hydrochloride aqueous solution at a bath ratio of 1:55, react at 50° C. for 3 h, and after the reaction is completed, take out the fabric, wash it with deionized water 5 times, and dry it at room temperature to obtain a modified pure cotton fabric; Step 5: Use the modified pure cotton fabric as the outer fabric and the inner fabric respectively, and use cotton thread to sew the outer fabric and the inner fabric of equal area to obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.
[0022] Comparative Example 2 This comparative example discloses a method for preparing an antibacterial, moisture-absorbing, breathable pure cotton fabric, comprising the following steps: Step 1, adding cotton fiber, ceric ammonium nitrate, and methacryloylethyl sulfonyl betaine to a 0.08 mol / L nitric acid aqueous solution, wherein the mass ratio of cotton fiber, ceric ammonium nitrate, methacryloylethyl sulfonyl betaine, and 0.08 mol / L nitric acid aqueous solution is 10:0.7:3:100, and reacting at 25°C for 3.5 hours under nitrogen protection. After the reaction is completed, taking out the cotton fiber, washing it thoroughly with deionized water to remove the initiator ceric ammonium nitrate, nitric acid, unreacted olefin-modified nano zinc oxide, and methacryloylethyl sulfonyl betaine on the surface of the cotton fiber, and obtaining a grafted cotton fiber; Step 2: First, the grafted cotton fiber is spun into pure cotton yarn with a yarn count of 40S. Then, the pure cotton yarn is spun into pure cotton fabric through a knitting process. The weight of the pure cotton fabric is 200g / m 2 ; Step 3: Immerse the pure cotton fabric in a 4 g / L polyhexamethyleneguanidine hydrochloride aqueous solution at a bath ratio of 1:55, react at 50° C. for 3 h, and after the reaction is completed, take out the fabric, wash it with deionized water 5 times, and dry it at room temperature to obtain a modified pure cotton fabric; Step 4: Use the modified pure cotton fabric as the outer fabric and the inner fabric respectively, and use cotton thread to sew the outer fabric and the inner fabric of equal area to obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.
[0023] Comparative Example 3 This comparative example discloses a method for preparing an antibacterial, moisture-absorbing, breathable pure cotton fabric, comprising the following steps: Step 1: dissolving dimethylaminoethyl methacrylate in methanol, adding chlorinated modified nano zinc oxide and potassium iodide, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, and methanol is 15.7:8.9:0.85:60, and reflux reaction at 65°C for 30 hours under nitrogen protection. After the reaction is completed, filtering, washing with ethanol 3 times, and placing in a vacuum drying oven at 60°C to dry to constant weight to obtain olefin-modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: : Add nano zinc oxide to ethanol, ultrasonicate at 50 kHz for 30 minutes, then add 3-chloropropyltrimethoxysilane, the mass ratio of nano zinc oxide, ethanol, and 3-chloropropyltrimethoxysilane is 8.1:250:20, react at 80°C for 40 minutes, add 2 mol / L hydrochloric acid aqueous solution to adjust the pH to 4, and continue to react at 80°C for 4 hours. After the reaction is completed, filter, wash with ethanol three times, and dry in a vacuum drying oven at 60°C to constant weight to obtain chloride-modified nano zinc oxide; Step 2, adding cotton fiber, ceric ammonium nitrate, alkenyl-modified nano zinc oxide, and methacryloylethyl sulfonyl betaine to a 0.08 mol / L nitric acid aqueous solution, wherein the mass ratio of cotton fiber, ceric ammonium nitrate, alkenyl-modified nano zinc oxide, methacryloylethyl sulfonyl betaine, sodium acetate, and 0.08 mol / L nitric acid aqueous solution is 10:0.7:2:3:1:100, and reacting at 25°C under nitrogen protection for 3.5 hours. After the reaction is completed, taking out the cotton fiber, washing it thoroughly with deionized water to remove the initiator ceric ammonium nitrate, nitric acid, and unreacted alkenyl-modified nano zinc oxide and methacryloylethyl sulfonyl betaine on the surface of the cotton fiber, to obtain a grafted cotton fiber; Step 3: First, the grafted cotton fiber is spun into pure cotton yarn with a yarn count of 40S. Then, the pure cotton yarn is spun into pure cotton fabric through a knitting process. The weight of the pure cotton fabric is 200g / m 2 ; Step 4: Use pure cotton fabrics as the outer fabric and the inner fabric respectively, and use cotton thread to sew the outer fabric and the inner fabric of equal area to obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.
[0024] In the above embodiments and comparative examples: dimethylaminoethyl methacrylate was purchased from Shanghai Xiangu Chemical Co., Ltd., CAS No.: 105-16-8; 3-chloropropyltrimethoxysilane was purchased from Guangzhou Shanghe Chemical Technology Co., Ltd., CAS No.: 2530-87-2; nano zinc oxide was purchased from Fujian Ruisen New Materials Co., Ltd., average particle size: 50nm; cotton fiber was purchased from Binzhou Shengchi Trading Co., Ltd., fiber length: 36mm; methacryloylethyl sulfobetaine was purchased from Jiangsu Leien Environmental Protection Technology Co., Ltd., CAS No.: 3637-26-1; polyhexamethyleneguanidine hydrochloride was purchased from Wuhan Kemik Biomedical Technology Co., Ltd., CAS No.: 32289-58-0; cotton thread was purchased from Shenzhen Shunlong Thread Co., Ltd., specification: 20S / 2.
[0025] Test Case The performance tests were conducted on the antibacterial, moisture-absorbing, and breathable pure cotton fabrics prepared in Examples 1-5 and Comparative Examples 1-3: (1) Moisture absorption and breathability: The moisture permeability of fabrics was measured with reference to the standard GB / T12704-2009 "Test method for moisture permeability of textile fabrics Part 1: Moisture absorption method", and the air permeability of fabrics was measured with reference to the standard GB / T5453-1997 "Determination of air permeability of textile fabrics". The test results are shown in Table 1:
[0026] As shown in Table 1, the pure cotton fabric prepared by the present invention has good moisture absorption and breathability. The present invention uses cotton fiber to prepare the fabric, which has good moisture absorption and breathability. The cotton fiber is subjected to a grafting modification treatment to introduce hydrophilic antibacterial components quaternary ammonium salt and betaine. The pure cotton fabric is subjected to antibacterial finishing and the hydrophilic guanidine salt is introduced. The introduction of hydrophilic groups can further improve the moisture absorption and breathability of the pure cotton fabric. Compared with Example 1, in Comparative Example 1, when preparing the grafted cotton fiber, methacryloylethyl sulfobetaine was not grafted, and without the introduction of betaine groups, the moisture absorption and breathability decreased. In Comparative Example 2, when preparing the grafted cotton fiber, alkenyl-modified nano zinc oxide was not grafted, and without the introduction of quaternary ammonium salt, the moisture absorption and breathability decreased. In Comparative Example 3, the pure cotton fabric did not undergo an antibacterial finishing reaction with the polyhexamethyleneguanidine hydrochloride aqueous solution, and without the introduction of guanidine salt, the moisture absorption and breathability also decreased.
[0027] (2) Antibacterial performance: The antibacterial rate of the fabric sample after washing 50 times was measured with reference to the standard FZ / T73023-2006 "Antibacterial Knitwear". The test results are shown in Table 2:
[0028] As shown in Table 2, the pure cotton fabric prepared by the present invention has good antibacterial properties. Dimethylaminoethyl methacrylate reacts with chlorinated modified nano zinc oxide under the action of potassium iodide catalyst to obtain olefin-modified nano zinc oxide, forming an antibacterial quaternary ammonium salt on the surface of the nano zinc oxide and introducing a carbon-carbon double bond; the carbon-carbon double bonds on the olefin-modified nano zinc oxide and methacryloylethyl sulfobetaine molecules undergo graft copolymerization with cotton fiber molecules, grafting the inorganic antibacterial component nano zinc oxide and the organic antibacterial component betaine onto the cotton fiber molecules, which can effectively improve the antibacterial properties of the cotton fiber; under the action of an initiator, free radicals capable of graft copolymerization with the carbon-carbon double bond are formed between the C2-C3 bonds of the cotton fiber molecular skeleton, while forming an aldehyde group, which can react with the amino group at the end of polyhexamethyleneguanidine hydrochloride, introducing antibacterial guanidine salt and forming a Schiff base, further improving the antibacterial properties. Compared with Example 1, when preparing the grafted cotton fiber in Comparative Example 1, methacryloylethyl sulfobetaine was not introduced, and the betaine group was not introduced, and the antibacterial property was reduced; when preparing the grafted cotton fiber in Comparative Example 2, olefin-modified nano-zinc oxide was not introduced, and the antibacterial property was also reduced; in Comparative Example 3, the pure cotton fabric did not undergo an antibacterial finishing reaction with the polyhexamethyleneguanidine hydrochloride aqueous solution, and the guanidine salt was not introduced, and the antibacterial property was also slightly reduced.
[0029] While embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions, and variations may be made to these embodiments without departing from the principles and spirit of the invention, and that the scope of the invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing antibacterial, moisture-absorbing and breathable pure cotton fabric, characterized in that: The following steps are involved: Step 1: dissolving dimethylaminoethyl methacrylate in methanol, adding chlorinated modified nano zinc oxide and potassium iodide, reacting, filtering, washing, and drying after the reaction is completed to obtain olefin-modified nano zinc oxide; Step 2: adding cotton fiber, cerium ammonium nitrate, alkenyl-modified nano zinc oxide, methacryloylethyl sulfobetaine and a buffer into a nitric acid aqueous solution, reacting, and after the reaction is completed, taking out, washing and drying to obtain grafted cotton fiber; Step 3: first spinning the grafted cotton fiber into pure cotton yarn, and then spinning the pure cotton yarn into pure cotton fabric through a knitting process; Step 4: soaking the pure cotton fabric in a polyhexamethyleneguanidine hydrochloride aqueous solution for reaction. After the reaction is completed, taking out, washing, and drying to obtain a modified pure cotton fabric; Step 5: Use the modified pure cotton fabric as the outer fabric and the inner fabric respectively, and compound the outer fabric and the inner fabric with equal areas to obtain an antibacterial, moisture-absorbing and breathable pure cotton fabric.
2. The method for preparing the antibacterial, moisture-absorbing, breathable pure cotton fabric according to claim 1, characterized in that: In the step 1, the mass ratio of dimethylaminoethyl methacrylate, chloride-modified nano-zinc oxide, potassium iodide, and methanol is 15.7:(8.9-9.3):(0.85-0.9):(60-80), and the reaction conditions are reflux reaction at 65-75° C. under nitrogen protection for 10-20 hours.
3. The method for preparing the antibacterial, moisture-absorbing, breathable pure cotton fabric according to claim 1, characterized in that: The chlorination-modified nano zinc oxide in step 1 is prepared by the following steps: adding nano zinc oxide to ethanol, ultrasonicating, adding 3-chloropropyltrimethoxysilane, reacting, adjusting the pH value to 4-5 after the reaction, continuing the reaction, filtering, washing, and drying to obtain chlorination-modified nano zinc oxide.
4. The method for preparing the antibacterial, moisture-absorbing, breathable pure cotton fabric according to claim 3, characterized in that: The mass ratio of nano zinc oxide, ethanol and 3-chloropropyltrimethoxysilane is 8.1:(250-300):(20-25). The reaction conditions are 80-90°C for 20-40 minutes and 80-90°C for 3-4 hours.
5. The method for preparing the antibacterial, moisture-absorbing and breathable pure cotton fabric according to claim 1, characterized in that: In the step 2, the mass ratio of cotton fiber, ammonium cerium nitrate, alkenyl-modified nano-zinc oxide, methacryloylethyl sulfobetaine, buffer and nitric acid aqueous solution is 10:(0.7-0.9):(2-4):(3-6):(0.5-2):(100-150), and the reaction conditions are under nitrogen protection and at a temperature of 25-35°C for 2.5-3.5 hours; the buffer is selected from one or a combination of acetic acid and sodium acetate, citric acid and sodium citrate, and is used to adjust the pH of the nitric acid aqueous solution to 4.0-5.5; the concentration of nitric acid in the nitric acid aqueous solution is 0.08-0.12 mol / L.
6. The method for preparing the antibacterial, moisture-absorbing and breathable pure cotton fabric according to claim 1, characterized in that: In step 3, the yarn count of the pure cotton yarn is 30-50S, and the weight of the pure cotton fabric is 180-220g / m 2 .
7. The method for preparing the antibacterial, moisture-absorbing and breathable pure cotton fabric according to claim 1, characterized in that: In the step 4, the bath ratio of the pure cotton fabric to the polyhexamethyleneguanidine hydrochloride aqueous solution is 1:(45-55), and the reaction conditions are 50-60° C. for 2-3 hours.
8. The method for preparing the antibacterial, moisture-absorbing and breathable pure cotton fabric according to claim 1, characterized in that: The concentration of polyhexamethyleneguanidine hydrochloride in the polyhexamethyleneguanidine hydrochloride aqueous solution in step 4 is 4-6 g / L.
9. An antibacterial, moisture-absorbing, breathable pure cotton fabric prepared by the method for preparing an antibacterial, moisture-absorbing, breathable pure cotton fabric according to any one of claims 1 to 8.
10. Use of the antibacterial, moisture-absorbing, breathable pure cotton fabric according to claim 9 in non-allergenic underwear.
Citation Information
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