Antibacterial moisture-absorbing and air-permeable pure cotton fabric, preparation method and application in non-allergic underwear

By grafting nano-zinc oxide and betaine onto cotton fibers and combining them with an antibacterial finishing reaction, the problem of insufficient antibacterial properties in pure cotton fabrics is solved, achieving highly efficient antibacterial, moisture-wicking, and breathable effects, making it suitable for non-allergenic underwear.

CN120680765BActive Publication Date: 2025-12-05GUANGDONG KINGFA MATERNITY & BABY PRODUCTS CO LTD
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Patent Information

Application Number
CN202510805255.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-06-17
Publication Date
2025-12-05
Estimated Expiration
2045-06-17

AI Technical Summary

Technical Problem

The antibacterial properties of existing pure cotton fabrics need to be improved, as they are prone to microbial growth, which can lead to skin allergic reactions.

Method used

By grafting and modifying cotton fibers, inorganic antibacterial component nano zinc oxide and organic antibacterial component betaine are introduced, and an air layer is formed through knitting process, which, combined with antibacterial finishing reaction, enhances antibacterial performance.

Benefits of technology

It significantly improves the antibacterial properties of cotton fibers, reduces skin irritation, and enhances moisture absorption, breathability, and warmth retention, making it suitable for hypoallergenic underwear.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application belongs to the technical field of fabrics, and particularly relates to an antibacterial moisture-absorbing and air-permeable pure cotton fabric, a preparation method and application in non-allergic underwear. The application uses cotton fibers to prepare the fabric, and the fabric has good moisture absorption and air permeability. Dimethylaminoethyl methacrylate reacts with chlorinated modified nano zinc oxide under the action of a catalyst potassium iodide to generate alkenyl modified nano zinc oxide. The alkenyl modified nano zinc oxide reacts with methacryloyl ethyl sulfobetaine under the action of a Ce(IV) salt initiator under acidic conditions, and graft copolymerization occurs with cotton fibers to obtain grafted cotton fibers. The cotton fibers are introduced with an antibacterial component through graft modification treatment, and the antibacterial performance can be effectively improved. The grafted cotton fibers are first spun into pure cotton yarn, and then spun into pure cotton fabric. The pure cotton fabric is subjected to antibacterial finishing of polyhexamethylene guanidine hydrochloride, and the antibacterial performance of the pure cotton fabric is further improved.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of fabrics, and particularly relates to an antibacterial moisture-absorbing and air-permeable pure cotton fabric, a preparation method and application in non-allergic underwear. BACKGROUND

[0002] The pure cotton fabric is prepared from natural plant fiber cotton fiber, has good warmth retention, soft hand feeling, good moisture absorption and air permeability, can reduce skin irritation and prevent skin allergy. During wearing, various secretions such as sweat and sebum in the human body can adhere to the fabric, which can provide a good living environment for various harmful microorganisms, promote the breeding and reproduction of microorganisms, and further cause skin allergy and other health problems. Therefore, the pure cotton fabric needs to be modified to have antibacterial properties to enhance the protection of the skin.

[0003] Chinese patent CN104264464B discloses a preparation method of organic cation modified textile fiber. Cotton fiber textile material is used as a carrier, and a quaternary ammonium compound containing active epoxy groups or dihydroxy groups is formed through a quaternary ammonium reaction between an organic cation precursor and epichlorohydrin, and then quaternary ammonium salt and quaternary phosphonium salt are grafted to the surface of the cotton fiber to form a cotton textile material with persistent antibacterial function. However, the molecular structure of cotton fiber is stable, and the number of active groups capable of grafting reaction with epoxy groups is limited, and the antibacterial performance needs to be improved. SUMMARY

[0004] The application provides an antibacterial moisture-absorbing and air-permeable pure cotton fabric to solve the problem of the need to improve the antibacterial performance of the pure cotton fabric in the prior art.

[0005] To achieve the above-mentioned purpose, the technical scheme adopted by the application is as follows: a preparation method of an antibacterial moisture-absorbing and air-permeable pure cotton fabric, comprising the following steps:

[0006] Step one, dimethylaminoethyl methacrylate is dissolved in methanol, chlorinated modified nano zinc oxide and potassium iodide are added, and then reacted. After the reaction is completed, the product is filtered, washed and dried to obtain alkenyl modified nano zinc oxide;

[0007] Step two, cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine and a buffer are added to an aqueous nitric acid solution, and then reacted. After the reaction is completed, the product is taken out, 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 aqueous nitric acid solution to 4.0-5.5;

[0008] Step three, the grafted cotton fiber is spun into pure cotton yarn, and then the pure cotton yarn is spun into pure cotton fabric through a knitting process;

[0009] Step four, immerse the pure cotton fabric in the aqueous solution of polyhexamethylene guanidine hydrochloride, react, after the reaction is completed, take out, wash, dry, and obtain the modified pure cotton fabric;

[0010] Step five, use the modified pure cotton fabric as the outer layer fabric and the inner layer fabric respectively, and composite the outer layer fabric and the inner layer fabric with equal area to obtain the antibacterial, moisture-absorbing and breathable pure cotton fabric.

[0011] Preferably, in the step one, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide and methanol is 15.7:(8.9-9.3):(0.85-0.9):(60-80), and the reaction condition is refluxing at 65-75℃ for 10-20h under nitrogen protection.

[0012] Preferably, the chlorinated modified nano zinc oxide is prepared by the following steps: adding nano zinc oxide into ethanol, after ultrasonic, adding 3-chloropropyl trimethoxysilane, reacting, after the reaction is completed, adjusting the pH value to 4-5, continuing to react, after the reaction is completed, filtering, washing, drying, and obtaining the chlorinated modified nano zinc oxide.

[0013] Preferably, the mass ratio of nano zinc oxide, ethanol and 3-chloropropyl trimethoxysilane is 8.1:(250-300):(20-25), and the reaction condition is reacting at 80-90℃ for 20-40min, and the continuing reaction condition is reacting at 80-90℃ for 3-4h.

[0014] Preferably, in the step two, the mass ratio of cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine, buffer and aqueous nitric acid solution is 10:(0.7-0.9):(2-4):(3-6):(0.5-2):(100-150), and the reaction condition is reacting at 25-35℃ for 2.5-3.5h under nitrogen protection; the buffer is selected from one or a combination of acetic acid and sodium acetate, citric acid and sodium citrate, which is used to adjust the pH of the aqueous nitric acid solution to 4.0-5.5; the concentration of nitric acid in the aqueous nitric acid solution is 0.08-0.12mol / L.

[0015] Preferably, in the step three, the yarn count of the pure cotton yarn is 30-50S (English count), and the grammage of the pure cotton fabric is 180-220g / m 2 .

[0016] Preferably, in the step four, the bath ratio of the pure cotton fabric to the aqueous solution of polyhexamethylene guanidine hydrochloride is 1:(45-55), and the reaction condition is reacting at 50-60℃ for 2-3h; the concentration of polyhexamethylene guanidine hydrochloride in the aqueous solution of polyhexamethylene guanidine hydrochloride is 4-6g / L.

[0017] The application further discloses a preparation method of the antibacterial moisture-absorbing and air-permeable pure cotton fabric.

[0018] The application further discloses application of the antibacterial moisture-absorbing and air-permeable pure cotton fabric in non-allergic underwear.

[0019] Compared with the prior art, the application has the following beneficial effects: the application uses cotton fibers to prepare the fabric, and the fabric has good moisture absorption and air permeability; the fabric comprises an inner layer fabric and an outer layer fabric, and the air layer formed through the gap between the two layer fabrics can improve the warmth retention performance of the fabric; the cotton fibers are subjected to grafting modification treatment, and inorganic antibacterial component nano zinc oxide and organic antibacterial component betaine are introduced, so that the antibacterial performance of the cotton fibers can be effectively improved; the pure cotton fabric spun from the grafted cotton fibers is subjected to antibacterial finishing, so that the antibacterial performance can be further improved; in the application, when the grafted cotton fibers are prepared, dimethylaminoethyl methacrylate is reacted with chlorinated modified nano zinc oxide under the action of a catalyst potassium iodide to obtain alkenyl modified nano zinc oxide, and at the same time, the antibacterial quaternary ammonium salt is formed on the surface of the nano zinc oxide, and the carbon-carbon double bond (-C=C-) is introduced; under the action of a Ce(IV) salt initiator, free radicals are formed between the C2-C3 bonds of the molecular skeleton of the cotton fibers under acidic conditions through a single electron transfer process, and then the grafting copolymerization reaction occurs between the free radicals and the carbon-carbon double bonds on the alkenyl modified nano zinc oxide and the methacryloyl ethyl sulfobetaine molecules, so that the inorganic antibacterial component nano zinc oxide and the organic antibacterial component betaine are grafted onto the cotton fibers, which can effectively improve the antibacterial performance of the cotton fibers, and the introduced betaine has an anti-allergic effect, which can reduce the irritation to the skin and prevent sensitization; in the application, when the grafted cotton fibers are prepared under the action of the initiator, the free radicals are formed between the C2-C3 bonds of the molecular skeleton of the cotton fibers at the same time, and aldehyde groups are formed; the pure cotton fabric is immersed in a polyhexamethylene guanidine hydrochloride aqueous solution to perform an antibacterial finishing reaction, the aldehyde groups can react with the amino groups at the end of the polyhexamethylene guanidine hydrochloride, the antibacterial guanidine salt is introduced onto the cotton fiber fabric through chemical bonding at the same time that the antibacterial Schiff base structure (-C=N-) is formed, and the antibacterial performance can be further improved; in addition, the antibacterial components quaternary ammonium salt, betaine and guanidine salt all have excellent hydrophilicity, which can further improve the moisture absorption and air permeability of the pure cotton fabric; and the pure cotton fabric is spun through a knitting process, and many small pores exist between the yarns, so that air can flow freely, thereby further improving the air permeability of the pure cotton fabric. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 A preparation process flow chart of the modified pure cotton fabric in the application is shown in the figure;

[0021] Figure 2A column chart of the moisture permeability test results of the antibacterial moisture-permeable and air-permeable pure cotton fabric prepared in the embodiments 1-5 and the comparative examples 1-3 of the present application;

[0022] Figure 3 A column chart of the air permeability test results of the antibacterial moisture-permeable and air-permeable pure cotton fabric prepared in the embodiments 1-5 and the comparative examples 1-3 of the present application;

[0023] Figure 4 A column chart of the antibacterial property test results of the antibacterial moisture-permeable and air-permeable pure cotton fabric prepared in the embodiments 1-5 and the comparative examples 1-3 of the present application. DETAILED DESCRIPTION

[0024] Embodiment 1

[0025] The present embodiment discloses a preparation method of an antibacterial moisture-permeable and air-permeable pure cotton fabric, comprising the following steps:

[0026] Step one, dimethylaminoethyl methacrylate is dissolved in methanol, chlorinated modified nano zinc oxide and potassium iodide are added, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, methanol is 15.7:8.9:0.85:60, under the protection of nitrogen, reflux reaction is carried out at 65℃ for 30h, after the reaction is completed, filtration is carried out, washing is carried out with ethanol for 3 times, drying is carried out in a vacuum drying box at 60℃ until the constant weight is obtained, to obtain alkenyl modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: nano zinc oxide is added into ethanol, after ultrasonic treatment at a frequency of 50kHz for 30min, 3-chloropropyl trimethoxysilane is added, the mass ratio of nano zinc oxide, ethanol, 3-chloropropyl trimethoxysilane is 8.1:250:20, after reaction at 80℃ for 40min, 2mol / L hydrochloric acid aqueous solution is added to adjust the pH value to 4, continuing to react at 80℃ for 4h, after the reaction is completed, filtration is carried out, washing is carried out with ethanol for 3 times, drying is carried out in a vacuum drying box at 60℃ until the constant weight is obtained, to obtain chlorinated modified nano zinc oxide;

[0027] Step two, cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine and a buffer are added into 0.08mol / L nitric acid aqueous solution, the mass ratio of cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine, buffer and 0.08mol / 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 1:1, to adjust the pH value of the nitric acid aqueous solution to 5.0; under the protection of nitrogen, reaction is carried out at 25℃ for 3.5h, after the reaction is completed, taking out, washing with deionized water to remove the initiator cerium ammonium nitrate, nitric acid, unreacted alkenyl modified nano zinc oxide and methacryloyl ethyl sulfobetaine on the surface of the cotton fiber, to obtain grafted cotton fiber;

[0028] Step three, first grafting cotton fibers into pure cotton yarn, the yarn count of pure cotton yarn is 40S, then pure cotton yarn is spun into pure cotton fabric by knitting process, the grammage of pure cotton fabric is 200g / m 2 ;

[0029] Step four, pure cotton fabric is immersed in 4g / L polyhexamethylene guanidine hydrochloride aqueous solution, the bath ratio of pure cotton fabric to 4g / L polyhexamethylene guanidine hydrochloride aqueous solution is 1:55, the reaction is carried out at 50℃ for 3h, after the reaction is completed, it is taken out, washed with deionized water for 5 times, and dried at room temperature to obtain modified pure cotton fabric;

[0030] Step five, the modified pure cotton fabric is used as the outer layer fabric and the inner layer fabric respectively, and the outer layer fabric and the inner layer fabric are sewn into a composite with equal area by using cotton thread to obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.

[0031] Example 2

[0032] The embodiment discloses a preparation method of antibacterial, moisture-absorbing and breathable pure cotton fabric, comprising the following steps:

[0033] Step one, dimethylaminoethyl methacrylate is dissolved in methanol, chlorinated modified nano zinc oxide and potassium iodide are added, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide and methanol is 15.7:9.3:0.9:80, the reflux reaction is carried out under nitrogen protection at 75℃ for 20h, after the reaction is completed, it is filtered, washed with ethanol for 3 times, and dried in a 60℃ vacuum drying box until the constant weight to obtain alkenyl modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: nano zinc oxide is added into ethanol, after ultrasonic treatment at 50kHz for 30min, 3-chloropropyltrimethoxysilane is added, the mass ratio of nano zinc oxide, ethanol and 3-chloropropyltrimethoxysilane is 8.1:300:25, after the reaction is carried out at 90℃ for 20min, 2mol / L hydrochloric acid aqueous solution is added to adjust the pH value to 5, and the reaction is continued at 90℃ for 3h, after the reaction is completed, it is filtered, washed with ethanol for 3 times, and dried in a 60℃ vacuum drying box until the constant weight to obtain chlorinated modified nano zinc oxide;

[0034] Step two, cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine are added into 0.12 mol / L nitric acid aqueous solution, the mass ratio of cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine, 0.12 mol / L nitric acid aqueous solution is 10:0.9:4:6:150, under nitrogen protection, at 35℃ for 2.5h, after the reaction is completed, take out, wash with deionized water to remove the initiator cerium ammonium nitrate on the surface of the cotton fiber, nitric acid, unreacted alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine, to obtain grafted cotton fiber;

[0035] Step three, first spin the grafted cotton fiber into pure cotton yarn, the yarn count of the pure cotton yarn is 40S, then spin the pure cotton yarn into pure cotton fabric through the knitting process, the grammage of the pure cotton fabric is 200g / m 2 ;

[0036] Step four, immerse the pure cotton fabric in 6g / L polyhexamethylene guanidine hydrochloride aqueous solution, the bath ratio of the pure cotton fabric to 6g / L polyhexamethylene guanidine hydrochloride aqueous solution is 1:45, react at 60℃ for 2h, after the reaction is completed, take out, wash with deionized water for 5 times, dry at room temperature, to obtain modified pure cotton fabric;

[0037] Step five, use the modified pure cotton fabric as the outer layer fabric and the inner layer fabric respectively, sew the outer layer fabric and the inner layer fabric with equal area to composite by cotton thread, to obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.

[0038] Example 3

[0039] The embodiment discloses a preparation method of antibacterial, moisture-absorbing and breathable pure cotton fabric, comprising the following steps:

[0040] Step one, dimethylaminoethyl methacrylate is dissolved in methanol, chlorinated modified nano zinc oxide and potassium iodide are added, and the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, methanol is 15.7:9:0.86:65, under the protection of nitrogen, reflux reaction at 70℃ for 24h, after the reaction is completed, filter, wash with ethanol for 3 times, place in 60℃ vacuum drying box to dry to constant weight, obtain alkenyl modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: nano zinc oxide is added into ethanol, ultrasonic at 50kHz frequency for 30min, then 3-chloropropyl trimethoxysilane is added, the mass ratio of nano zinc oxide, ethanol, 3-chloropropyl trimethoxysilane is 8.1:260:21, after reaction at 85℃ for 30min, 2mol / L hydrochloric acid aqueous solution is added to adjust pH value to 4.5, continue to react at 85℃ for 3.5h, after the reaction is completed, filter, wash with ethanol for 3 times, place in 60℃ vacuum drying box to dry to constant weight, obtain chlorinated modified nano zinc oxide;

[0041] Step two, cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine are added into 0.09mol / L nitric acid aqueous solution, the mass ratio of cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine, 0.09mol / L nitric acid aqueous solution is 10:0.75:2.5:4:110, under the protection of nitrogen, react at 30℃ for 3h, after the reaction is completed, take out, wash with deionized water to remove the initiator cerium ammonium nitrate, nitric acid, unreacted alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine on the surface of cotton fiber, obtain grafted cotton fiber;

[0042] Step three, first spin the grafted cotton fiber into pure cotton yarn, the yarn count of pure cotton yarn is 40S, then spin the pure cotton yarn into pure cotton fabric by knitting process, the grammage of pure cotton fabric is 200g / m 2 ;

[0043] Step four, immerse the pure cotton fabric in 4.5g / L polyhexamethylene guanidine hydrochloride aqueous solution, the bath ratio of pure cotton fabric and 4.5g / L polyhexamethylene guanidine hydrochloride aqueous solution is 1:50, react at 55℃ for 2.5h, after the reaction is completed, take out, wash with deionized water for 5 times, dry at room temperature, obtain modified pure cotton fabric;

[0044] Step five, take the modified pure cotton fabric as outer layer fabric and inner layer fabric respectively, sew the outer layer fabric and the inner layer fabric into composite with equal area by cotton thread, obtain antibacterial moisture-absorbing and air-permeable pure cotton fabric.

[0045] Example 4

[0046] The embodiment discloses a preparation method of antibacterial moisture-absorbing and air-permeable pure cotton fabric, and comprises the following steps:

[0047] Step one, dimethylaminoethyl methacrylate is dissolved in methanol, chlorinated modified nano zinc oxide and potassium iodide are added, and the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, methanol is 15.7:9.1:0.87:70, under the protection of nitrogen, reflux reaction is carried out at 70 DEG C for 24 hours, after the reaction is completed, filtration is carried out, washing is carried out three times with ethanol, and drying is carried out in a vacuum drying box at 60 DEG C until the constant weight is obtained, thereby obtaining alkenyl modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: nano zinc oxide is added into ethanol, ultrasonic treatment is carried out at a frequency of 50 kHz for 30 min, then 3-chloropropyl trimethoxysilane is added, the mass ratio of nano zinc oxide, ethanol and 3-chloropropyl trimethoxysilane is 8.1:275:22.5, after reaction is carried out at 85 DEG C for 30 min, 2 mol / L hydrochloric acid aqueous solution is added to adjust the pH value to 4.5, and then continuous reaction is carried out at 85 DEG C for 3.5 hours, after the reaction is completed, filtration is carried out, washing is carried out three times with ethanol, and drying is carried out in a vacuum drying box at 60 DEG C until the constant weight is obtained, thereby obtaining chlorinated modified nano zinc oxide;

[0048] Step two, cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide and methacryloyl ethyl sulfobetaine are added into 0.1 mol / L nitric acid aqueous solution, the mass ratio of cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine and 0.1 mol / L nitric acid aqueous solution is 10:0.8:3:4.5:125, reaction is carried out at 30 DEG C for 3 hours under the protection of nitrogen, after the reaction is completed, the grafting cotton fiber is obtained by taking out and washing with deionized water to remove the initiator cerium ammonium nitrate, nitric acid, unreacted alkenyl modified nano zinc oxide and methacryloyl ethyl sulfobetaine on the surface of the cotton fiber;

[0049] Step three, the grafting cotton fiber is first spun into pure cotton yarn, the yarn count of the pure cotton yarn is 40S, then the pure cotton yarn is spun into pure cotton fabric through a knitting process, and the grammage of the pure cotton fabric is 200 g / m 2 ;

[0050] Step four, the pure cotton fabric is immersed in 5 g / L polyhexamethylene guanidine hydrochloride aqueous solution, the bath ratio of the pure cotton fabric and the 5 g / L polyhexamethylene guanidine hydrochloride aqueous solution is 1:50, reaction is carried out at 55 DEG C for 2.5 hours, after the reaction is completed, the modified pure cotton fabric is obtained by taking out, washing five times with deionized water and air drying at room temperature;

[0051] Step five, the modified pure cotton fabric is used as the outer layer fabric and the inner layer fabric respectively, the outer layer fabric and the inner layer fabric are sewn together in equal area by using cotton thread, and the antibacterial moisture-absorbing and air-permeable pure cotton fabric is obtained.

[0052] Example 5

[0053] The embodiment discloses a preparation method of an antibacterial moisture-absorbing and air-permeable pure cotton fabric, and comprises the following steps:

[0054] Step one, dimethylaminoethyl methacrylate is dissolved in methanol, chlorinated modified nano zinc oxide and potassium iodide are added, and the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, methanol is 15.7:9.2:0.88:75, under the protection of nitrogen, reflux reaction is carried out at 70 DEG C for 24 hours, after the reaction is completed, filtration is carried out, washing is carried out with ethanol for three times, and drying is carried out in a vacuum drying box at 60 DEG C until the constant weight is obtained, and alkenyl modified nano zinc oxide is obtained; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: nano zinc oxide is added into ethanol, ultrasonic treatment is carried out at a frequency of 50 kHz for 30 min, then 3-chloropropyl trimethoxysilane is added, the mass ratio of nano zinc oxide, ethanol and 3-chloropropyl trimethoxysilane is 8.1:290:24, after reaction is carried out at 85 DEG C for 30 min, 2 mol / L hydrochloric acid aqueous solution is added to adjust the pH value to 4.5, and the reaction is continuously carried out at 85 DEG C for 3.5 h, after the reaction is completed, filtration is carried out, washing is carried out with ethanol for three times, and drying is carried out in a vacuum drying box at 60 DEG C until the constant weight is obtained, and chlorinated modified nano zinc oxide is obtained;

[0055] Step two, cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide and methacryloyl ethyl sulfobetaine are added into 0.11 mol / L nitric acid aqueous solution, the mass ratio of cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine and 0.11 mol / L nitric acid aqueous solution is 10:0.85:3.5:5:140, reaction is carried out at 30 DEG C for 3 h under the protection of nitrogen, after the reaction is completed, the initiator cerium ammonium nitrate, nitric acid, unreacted alkenyl modified nano zinc oxide and methacryloyl ethyl sulfobetaine on the surface of the cotton fiber are removed by taking out and washing with deionized water, and grafted cotton fiber is obtained;

[0056] Step three, the grafted cotton fiber is spun into pure cotton yarn, the yarn count of the pure cotton yarn is 40S, and then the pure cotton yarn is spun into a pure cotton fabric through a knitting process, and the grammage of the pure cotton fabric is 200 g / m 2 ;

[0057] Step four, the pure cotton fabric is immersed in 5.5 g / L polyhexamethylene guanidine hydrochloride aqueous solution, the bath ratio of the pure cotton fabric and the 5.5 g / L polyhexamethylene guanidine hydrochloride aqueous solution is 1:50, reaction is carried out at 55 DEG C for 2.5 h, after the reaction is completed, the pure cotton fabric is taken out and washed with deionized water for five times, and is dried at room temperature, and a modified pure cotton fabric is obtained;

[0058] Step five, the modified pure cotton fabric is used as the outer layer fabric and the inner layer fabric respectively, the outer layer fabric and the inner layer fabric are sewn together by using cotton thread, and an antibacterial and moisture-absorbing and air-permeable pure cotton fabric is obtained.

[0059] Comparative example 1

[0060] The comparative example discloses a preparation method of an antibacterial and moisture-absorbing and air-permeable pure cotton fabric, comprising the following steps:

[0061] Step one, dimethylaminoethyl methacrylate is dissolved in methanol, chlorinated modified nano zinc oxide and potassium iodide are added, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide and methanol is 15.7:8.9:0.85:60, reflux reaction is carried out under nitrogen protection at 65℃ for 30h, after the reaction is completed, filtration is carried out, washing is carried out with ethanol for 3 times, and drying is carried out in a vacuum drying box at 60℃ until the constant weight is obtained, and alkenyl modified nano zinc oxide is obtained; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: nano zinc oxide is added into ethanol, ultrasonic treatment is carried out at 50kHz for 30min, 3-chloropropyl trimethoxysilane is added, the mass ratio of nano zinc oxide, ethanol and 3-chloropropyl trimethoxysilane is 8.1:250:20, reaction is carried out at 80℃ for 40min, 2mol / L hydrochloric acid aqueous solution is added to adjust the pH value to 4, and reaction is continued at 80℃ for 4h, after the reaction is completed, filtration is carried out, washing is carried out with ethanol for 3 times, and drying is carried out in a vacuum drying box at 60℃ until the constant weight is obtained, and chlorinated modified nano zinc oxide is obtained;

[0062] Step two, cotton fiber, cerium ammonium nitrate and alkenyl modified nano zinc oxide are added into 0.08mol / L nitric acid aqueous solution, the mass ratio of cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide and 0.08mol / L nitric acid aqueous solution is 10:0.7:2:100, reaction is carried out under nitrogen protection at 25℃ for 3.5h, after the reaction is completed, the grafting cotton fiber is obtained by taking out and washing with deionized water to remove the initiator cerium ammonium nitrate, nitric acid, unreacted alkenyl modified nano zinc oxide and methacryloyl ethyl sulfobetaine on the surface of the cotton fiber;

[0063] Step three, the grafting cotton fiber is spun into pure cotton yarn, the yarn count of the pure cotton yarn is 40S, and the pure cotton yarn is spun into pure cotton fabric through a knitting process, and the grammage of the pure cotton fabric is 200g / m 2 ;

[0064] Step four, the pure cotton fabric is immersed in 4g / L polyhexamethylene guanidine hydrochloride aqueous solution, the bath ratio of the pure cotton fabric and the 4g / L polyhexamethylene guanidine hydrochloride aqueous solution is 1:55, reaction is carried out at 50℃ for 3h, after the reaction is completed, the modified pure cotton fabric is obtained by taking out, washing with deionized water for 5 times and air drying at room temperature;

[0065] Step five, the modified pure cotton fabric is used as the outer layer fabric and the inner layer fabric respectively, the outer layer fabric and the inner layer fabric are sewn and compounded by using cotton thread, and an antibacterial, moisture-absorbing and breathable pure cotton fabric is obtained.

[0066] Comparative example 2

[0067] The comparative example discloses a preparation method of an antibacterial, moisture-absorbing and breathable pure cotton fabric, comprising the following steps:

[0068] Step one, cotton fibers, cerium ammonium nitrate and methacryloyl ethyl sulfobetaine are added into 0.08 mol / L nitric acid aqueous solution, the mass ratio of the cotton fibers, the cerium ammonium nitrate, the methacryloyl ethyl sulfobetaine and the 0.08 mol / L nitric acid aqueous solution is 10:0.7:3:100, the reaction is carried out under nitrogen protection at 25 DEG C for 3.5 h, after the reaction is completed, the grafting cotton fibers are taken out and washed with deionized water to remove the initiator cerium ammonium nitrate, nitric acid, unreacted alkenyl modified nano zinc oxide and methacryloyl ethyl sulfobetaine on the surface of the cotton fibers, and the grafting cotton fibers are obtained;

[0069] Step two, the grafting cotton fibers are spun into pure cotton yarn, the yarn count of the pure cotton yarn is 40S, and then the pure cotton yarn is spun into a pure cotton fabric by using a knitting process, and the grammage of the pure cotton fabric is 200 g / m 2 ;

[0070] Step three, the pure cotton fabric is immersed in 4 g / L polyhexamethylene guanidine hydrochloride aqueous solution, the bath ratio of the pure cotton fabric to the 4 g / L polyhexamethylene guanidine hydrochloride aqueous solution is 1:55, the reaction is carried out at 50 DEG C for 3 h, after the reaction is completed, the modified pure cotton fabric is taken out, washed with deionized water for 5 times and dried at room temperature.

[0071] Step four, the modified pure cotton fabric is used as the outer layer fabric and the inner layer fabric respectively, the outer layer fabric and the inner layer fabric are sewn and compounded by using cotton thread, and an antibacterial, moisture-absorbing and breathable pure cotton fabric is obtained.

[0072] Comparative example 3

[0073] The comparative example discloses a preparation method of an antibacterial, moisture-absorbing and breathable pure cotton fabric, comprising the following steps:

[0074] Step one, dimethylaminoethyl methacrylate is dissolved in methanol, chlorinated modified nano zinc oxide and potassium iodide are added, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide, methanol is 15.7:8.9:0.85:60, under the protection of nitrogen, reflux reaction at 65℃ for 30h, after the reaction is completed, filter, wash with ethanol for 3 times, place in a vacuum drying oven at 60℃ to dry to constant weight, obtain alkenyl modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: nano zinc oxide is added into ethanol, after ultrasonic treatment at 50kHz for 30min, 3-chloropropyltrimethoxysilane is added, the mass ratio of nano zinc oxide, ethanol, 3-chloropropyltrimethoxysilane is 8.1:250:20, after reaction at 80℃ for 40min, 2mol / L hydrochloric acid aqueous solution is added to adjust the pH value to 4, continue to react at 80℃ for 4h, after the reaction is completed, filter, wash with ethanol for 3 times, place in a vacuum drying oven at 60℃ to dry to constant weight, obtain chlorinated modified nano zinc oxide;

[0075] Step two, cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine are added into 0.08mol / L nitric acid aqueous solution, the mass ratio of cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine, sodium acetate, 0.08mol / L nitric acid aqueous solution is 10:0.7:2:3:1:100, under the protection of nitrogen, react at 25℃ for 3.5h, after the reaction is completed, take out, wash with deionized water to remove the initiator cerium ammonium nitrate, nitric acid, unreacted alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine on the surface of cotton fiber, obtain grafted cotton fiber;

[0076] Step three, first spin the grafted cotton fiber into pure cotton yarn, the yarn count of pure cotton yarn is 40S, then spin the pure cotton yarn into pure cotton fabric by knitting process, the grammage of pure cotton fabric is 200g / m 2 ;

[0077] Step four, take pure cotton fabric as outer layer fabric and inner layer fabric respectively, sew the outer layer fabric and the inner layer fabric into composite with equal area by cotton thread, obtain antibacterial, moisture-absorbing and breathable pure cotton fabric.

[0078] In the above examples and comparative examples: dimethylaminoethyl methacrylate was purchased from Shanghai Xianggu Chemical Co., Ltd., CAS No.: 105-16-8; 3-chloropropyl trimethoxysilane was purchased from Guangzhou Shanghe Chemical Technology Co., Ltd., CAS No.: 2530-87-2; nano zinc oxide was purchased from Fujian Ruisen New Material Co., Ltd., average particle size: 50 nm; cotton fiber was purchased from Binzhou Shengchi Business and Trade Co., Ltd., fiber length: 36 mm; methacryloyl ethyl sulfobetaine was purchased from Jiangsu Lein Environmental Protection Technology Co., Ltd., CAS No.: 3637-26-1; polyhexamethylene guanidine hydrochloride was purchased from Wuhan Kemik Biological Medicine Technology Co., Ltd., CAS No.: 32289-58-0; cotton thread was purchased from Shenzhen Shunlong Thread Co., Ltd., specification: 20S / 2.

[0079] Test examples

[0080] The antibacterial moisture-permeable pure cotton fabric prepared in examples 1-5 and comparative examples 1-3 was subjected to performance testing:

[0081] (1) Moisture-permeability: the moisture permeability of the fabric was determined according to the standard GB / T12704-2009 “Textiles - Determination of water vapour transmission - Part 1: water vapour permeability test by the moisture method”, and the air permeability of the fabric was determined according to the standard GB / T5453-1997 “Textiles - Determination of air permeability of fabrics”, and the test results are shown in Table 1:

[0082]

[0083] As shown in Table 1, the pure cotton fabric prepared by the present application has good moisture-permeability. The cotton fiber is used to prepare the fabric, which has good moisture absorption and air permeability; the cotton fiber is subjected to grafting modification treatment, and hydrophilic antibacterial components quaternary ammonium salt and betaine are introduced, the pure cotton fabric is subjected to antibacterial finishing, and hydrophilic guanidine salt is introduced, and the introduction of hydrophilic groups can further improve the moisture-permeability of the pure cotton fabric. Compared with example 1, in comparative example 1, the grafted cotton fiber was prepared without the introduction of methacryloyl ethyl sulfobetaine, and the introduction of betaine groups was not introduced, and the moisture-permeability was decreased; in comparative example 2, the grafted cotton fiber was prepared without the introduction of alkenyl modified nano zinc oxide, and the introduction of quaternary ammonium salt was not introduced, and the moisture-permeability was decreased; in comparative example 3, the pure cotton fabric was not subjected to antibacterial finishing reaction with polyhexamethylene guanidine hydrochloride aqueous solution, and the introduction of guanidine salt was not introduced, and the moisture-permeability was also decreased.

[0084] (2) Antibacterial performance: the antibacterial rate of the fabric sample after 50 times of washing was determined according to the standard FZ / T73023-2006 “Antibacterial Knitted Fabrics”, and the determination results are shown in Table 2:

[0085]

[0086] It can be seen from Table 2 that the pure cotton fabric prepared by the application has good antibacterial performance. The alkenyl modified nano zinc oxide is obtained by reacting dimethylaminoethyl methacrylate with chlorinated modified nano zinc oxide under the action of a catalyst potassium iodide, an antibacterial quaternary ammonium salt is formed on the surface of the nano zinc oxide, and a carbon-carbon double bond is introduced; the alkenyl modified nano zinc oxide and the carbon-carbon double bond on the molecule of the methacryloyl ethyl sulfobetaine are grafted and copolymerized with the cotton fiber molecules, the inorganic antibacterial component nano zinc oxide and the organic antibacterial component betaine are grafted onto the cotton fiber molecules, and the antibacterial performance of the cotton fiber can be effectively improved; under the action of the initiator, the free radicals capable of grafting and copolymerizing with the carbon-carbon double bond are formed between the C2-C3 bonds of the cotton fiber molecular skeleton at the same time, and the aldehyde group is formed, which can react with the amino group at the end of the polyhexamethylene guanidine hydrochloride, the antibacterial guanidine salt is introduced at the same time, the Schiff base is formed, and the antibacterial performance is further improved. Compared with Example 1, in Comparative Example 1, the grafted cotton fiber is prepared without introducing the methacryloyl ethyl sulfobetaine, and the antibacterial performance is reduced due to the absence of the introduction of the betaine group; in Comparative Example 2, the grafted cotton fiber is prepared without introducing the alkenyl modified nano zinc oxide, and the antibacterial performance is also reduced due to the absence of the introduction of the nano zinc oxide and the quaternary ammonium salt; in Comparative Example 3, the pure cotton fabric is not subjected to the antibacterial finishing reaction with the aqueous solution of polyhexamethylene guanidine hydrochloride, and the antibacterial performance is also slightly reduced due to the absence of the introduction of the guanidine salt.

[0087] Although the embodiments of the application have been shown and described, it is to be understood that for the purpose of the present application, the changes, modifications, equivalents, substitutions and variations of the embodiments can be made by those skilled in the art without departing from the spirit and principles of the application, and the scope of the application is defined by the appended claims and their equivalents.

Claims

1. A method for preparing an antibacterial moisture-absorbing and air-permeable pure cotton fabric, characterized by, It comprises the following steps: Step one, dimethylaminoethyl methacrylate is dissolved in methanol, chlorinated modified nano zinc oxide and potassium iodide are added, and then the mixture is reacted, after the reaction is completed, the mixture is filtered, washed and dried to obtain the alkenyl modified nano zinc oxide; wherein, the chlorinated modified nano zinc oxide is prepared by the following steps: nano zinc oxide is added into ethanol, after ultrasonic treatment, 3-chloropropyltrimethoxysilane is added, and then the mixture is reacted, after the reaction is completed, the pH value is adjusted to 4-5, and then the mixture is continuously reacted, after the reaction is completed, the mixture is filtered, washed and dried to obtain the chlorinated modified nano zinc oxide; Step two, cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine and a buffer are added into an aqueous nitric acid solution, and then the mixture is reacted, after the reaction is completed, the mixture is taken out, washed and dried to obtain the grafted cotton fiber; Step three, the grafted cotton fiber is first spun into pure cotton yarn, and then the pure cotton yarn is spun into pure cotton fabric through a knitting process; Step four, the pure cotton fabric is immersed in an aqueous solution of polyhexamethylene guanidine hydrochloride, and then the mixture is reacted, after the reaction is completed, the mixture is taken out, washed and dried to obtain the modified pure cotton fabric; Step five, the modified pure cotton fabric is used as the outer layer fabric and the inner layer fabric respectively, the outer layer fabric and the inner layer fabric are compounded in equal area to obtain the antibacterial, moisture-absorbing and air-permeable pure cotton fabric.

2. The method for preparing the antibacterial, moisture-wicking, and breathable pure cotton fabric according to claim 1, characterized in that, In step one, the mass ratio of dimethylaminoethyl methacrylate, chlorinated modified nano zinc oxide, potassium iodide and methanol is 15.7:(8.9-9.3):(0.85-0.9):(60-80), and the reaction condition is refluxing at 65-75℃ for 10-20h under nitrogen protection.

3. The method for preparing the antibacterial, moisture-wicking, and breathable pure cotton fabric according to claim 1, characterized in that, In step one, when preparing the chlorinated modified nano zinc oxide, the mass ratio of nano zinc oxide, ethanol and 3-chloropropyltrimethoxysilane is 8.1:(250-300):(20-25), and the reaction condition is 80-90℃ for 20-40min, and the continuous reaction condition is 80-90℃ for 3-4h.

4. The method for preparing the antibacterial, moisture-wicking, and breathable pure cotton fabric according to claim 1, characterized in that, In step two, the mass ratio of cotton fiber, cerium ammonium nitrate, alkenyl modified nano zinc oxide, methacryloyl ethyl sulfobetaine, buffer and aqueous nitric acid solution is 10:(0.7-0.9):(2-4):(3-6):(0.5-2):(100-150), and the reaction condition is 25-35℃ for 2.5-3.5h under nitrogen protection; 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 aqueous nitric acid solution to 4.0-5.5; The concentration of nitric acid in the aqueous nitric acid solution is 0.08-0.12mol / L.

5. The method of preparing an anti-bacterial, moisture-absorbing, and air-permeable pure cotton fabric according to claim 1, characterized in that, In the third step, the yarn count of the pure cotton yarn is 30-50S, and the grammage of the pure cotton fabric is 180-220g / m 2 .

6. The method of producing an anti-bacterial moisture absorbing and vapor permeable pure cotton fabric according to claim 1, characterized in that, In step four, the bath ratio of pure cotton fabric to aqueous solution of polyhexamethylene guanidine hydrochloride is 1:(45-55), and the reaction condition is 50-60℃ for 2-3h.

7. The method of producing an anti-bacterial moisture absorption and air permeation pure cotton fabric according to claim 1, characterized in that, The concentration of polyhexamethylene guanidine hydrochloride in the aqueous solution of polyhexamethylene guanidine hydrochloride in step four is 4-6g / L. 8.An antibacterial, moisture-absorbing and air-permeable pure cotton fabric prepared by the preparation method of the antibacterial, moisture-absorbing and air-permeable pure cotton fabric according to any one of claims 1-7.

9. Use of the antibacterial moisture-absorbing and air-permeable pure cotton fabric according to claim 8 in non-allergic underwear.

Citation Information

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