Skin-friendly textile with antibacterial function and preparation method thereof

Through copolymer monomer solution impregnation, irradiation and halogenation treatment, the problems of high cost and poor durability in the preparation of existing antibacterial textiles are solved, and low-cost and efficient antibacterial functional coating preparation is achieved, which is suitable for a variety of textiles.

CN117802781BActive Publication Date: 2025-10-03GUANGDONG IND TECHN COLLEGE
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Patent Information

Application Number
CN202210309087.5
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-03-28
Publication Date
2025-10-03
Estimated Expiration
2042-03-28

AI Technical Summary

Technical Problem

Existing methods for preparing antibacterial textiles have problems such as high cost, poor durability, and difficulty in uniform penetration of finishing liquids, especially on non-degreased and water-resistant fabrics, which affects the antibacterial effect and production efficiency.

Method used

The textiles are impregnated with a solution of ethanol, diallylamine and a second monomer copolymer, combined with irradiation treatment and supercritical CO2 extraction technology, and then halogenated in a halide solution with a specific pH value and concentration to form a copolymer coating with antibacterial function.

Benefits of technology

The low-cost and efficient preparation of antibacterial functional coatings is achieved, which ensures the skin-friendliness and antibacterial effect of the fabric, avoids the environmental pollution of small molecule antibacterial agents, and is suitable for a variety of textiles, including hats, clothing, underwear, etc.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides a skin-friendly textile with antibacterial function and a preparation method thereof. The method comprises the following steps: A. sequentially adding ethanol, diallylamine, and a second monomer, stirring and mixing to form an impregnation solution, wherein the diallylamine is added in an amount of 30.0-60.0% by mass of the comonomer, and the second monomer is one of N,N-diethylacrylamide or N,N-dimethylacrylamide, or a mixture of the two; B. impregnation and finishing; C. drying; D. irradiation; E. extraction; and F. halogenation. The present invention is a textile with antibacterial function. The fiber fabric thereof not only serves as a textile but also as a carrier for antibacterial and sterilizing compounds, thereby achieving antibacterial and sterilizing purposes without causing secondary pollution to the environment, thereby achieving a safe and environmentally friendly antibacterial purpose.
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Description

Technical Field

[0001] The invention belongs to the technical field of antibacterial materials, and in particular relates to a method for preparing antibacterial fabric. Background Art

[0002] With the frequent occurrence of global acute infectious disease outbreaks, especially the further spread of COVID-19 around the world, people's awareness of personal protection has been increasing. How to effectively inhibit the growth of harmful bacteria and then completely eliminate them has received increasing attention from scholars. Textiles are the most important protective materials that isolate the human body from the external environment. Their rich loose porous structure and large specific surface area make them extremely easy to absorb large amounts of oil and sweat secreted during the human body's metabolism, providing a breeding ground for the attachment, breeding and massive reproduction of microorganisms. The large-scale proliferation of harmful pathogens on the surface of textiles not only produces odor, but also indirectly spreads diseases in some public places such as hospitals, hotels, and bathrooms, posing a safety hazard to human health. Therefore, the development of functional textiles, especially functional antibacterial textiles, is imminent.

[0003] Functional antimicrobial textiles are novel textile materials that effectively inhibit or kill microorganisms, such as bacteria and fungi, and offer health and hygiene benefits. They not only effectively prevent the spread of disease and infection, but also significantly reduce the risk of cross-infection in public environments. Currently, there are numerous types of antimicrobial textiles, primarily classified into two categories based on their preparation methods: co-spinning and finishing. Co-spinning involves uniformly mixing antimicrobial particles with a spinning matrix, spinning the mixture, and then producing the textile. However, antimicrobial particles are expensive and relatively large in size, making them difficult to disperse. During the spinning process, the particles can easily clog the spinnerets and break the yarns, leading to frequent failures and directly impacting normal production. These textiles are therefore only suitable for chemical spinning. They cannot process native plant fibers such as cotton, linen, and silk. Another type of antimicrobial textile is the post-finishing process using antimicrobial agents. This involves treating the fabric with an antimicrobial finish during the finishing process to impart antimicrobial properties. This processing method is mature and simple, offering flexibility in product variety and process changes, but suffers from relatively poor durability. At the same time, in the post-finishing method, the processing medium is water. However, for fabrics used in winter, especially non-degreased and water-resistant fabrics such as down jackets, cotton jackets, cotton quilts, etc., it is difficult for the finishing liquid to penetrate evenly during the finishing process.

[0004] Therefore, it is of great significance to develop a post-antibacterial finishing method for non-degreased fabrics with certain water resistance. Summary of the Invention

[0005] In view of the shortcomings of existing antibacterial functional textiles and preparation methods thereof, the object of the present invention is to provide a preparation method of skin-friendly textiles with antibacterial function.

[0006] In order to achieve the above object, the present invention adopts the following technical solutions:

[0007] A method for preparing skin-friendly textiles with antibacterial function, comprising the following steps: A. preparing an impregnation liquid:

[0008] In the reactor, ethanol, diallylamine, and the second monomer are added in sequence and stirred and mixed. The amount of ethanol is adjusted to prepare a solution with a comonomer concentration of 5.0-10.0%. The mixture is stirred and mixed until the impregnation solution is obtained. The amount of diallylamine added is 30.0-60.0% of the mass fraction of the comonomer. The second monomer is N,N-diethylacrylamide or N,N-dimethylacrylamide, or a mixture of the two. B. Impregnation Finishing:

[0009] Then, the impregnation liquid is used to impregnate the textiles through an impregnation and de-impregnation device to obtain impregnated textiles, with a rolling rate of 20-120%. The concentration of the impregnation liquid is adjusted according to 0.01-3.0% of the absolute dry mass of the comonomer absorbed by the textiles.

[0010] The immersion and dehydration equipment comprises an immersion tank for immersion and a dehydration machine for dehydration.

[0011] C. Drying:

[0012] The impregnated textiles that have been impregnated and finished are dried to remove the ethanol to obtain dried textiles.

[0013] D. Irradiation: Then, the dried textiles are irradiated in a controlled atmosphere to obtain irradiated textiles.

[0014] E. Extraction:

[0015] The irradiated textile and the entrainer are then placed together in an extraction kettle of a supercritical extraction device. Unreacted monomers are dissolved by extraction with CO2 in a supercritical state, and the unreacted monomers are separated in a separation kettle to remove the unreacted residual monomers to obtain an extracted textile. The entrainer is a solvent that has good solubility in the residual monomers, selected from ethanol, methanol, or a mixture of the two, preferably ethanol. The amount of the entrainer is 5.0 to 40.0% of the mass fraction of CO2.

[0016] F. Halogenation:

[0017] The extracted textile treated above is immersed in an aqueous hypohalite solution having a pH value of 6.5 to 7.5 and a mass percentage concentration of 0.1 to 10.0%, and a halogenation reaction is carried out at room temperature for 30 to 80 minutes. The textile is then taken out for dehydration and dried at a temperature of 40 to 50° C. to obtain a skin-friendly textile with antibacterial function, the surface of which is coated with an N-halodiallylamine copolymer having a structure represented by general formula (I).

[0018]

[0019] In formula (I), X represents a halogen atom such as chlorine or bromine, preferably a chlorine atom; and n represents the degree of polymerization.

[0020] As an optional method, in the preparation of the impregnation solution in step A, in the reactor, while diallylamine and the second monomer are added in sequence, a cross-linking agent monomer with cross-linking properties can also be added, and the added amount is 0.01 to 30.0% of the mass fraction of the comonomer, preferably 3.0% to 20.0%, and more preferably 3.0% to 10.0%.

[0021] The crosslinking monomer is a monomer or oligomer having two or more vinyl groups, including diisopropenylbenzene, divinylbenzene, triallylamine, methylenebisacrylamide, ethylene glycol diacrylate, ethylene glycol dimethacrylate, diethylene glycol diacrylate, triethylene glycol diacrylate, 1,4-butanediol diacrylate, trimethylolpropane triacrylate, pentaerythritol triacrylate, etc., selected from one or a mixture of two or more thereof, preferably methylenebisacrylamide and divinylbenzene.

[0022] As a preferred embodiment, the added amount of diallylamine is 45.0 to 52.5% of the mass fraction of the comonomer.

[0023] Preferably, the irradiation treatment in step D involves irradiating the dried textile with an electron beam accelerator at a dose of 10 to 150 kGy, preferably 20 to 60 kGy. The controlled atmosphere treatment is achieved by replacing the air in the process environment with nitrogen or carbon dioxide at a certain pressure, or a mixture thereof. The certain pressure refers to a relative pressure greater than 0.0 MPa, preferably 0.01 to 0.15 MPa.

[0024] Specifically, the electron beam accelerator is a high-energy electron beam accelerator, including a high-voltage accelerator, an induction accelerator, and a resonant accelerator.

[0025] Specifically, the hypohalite in step F is selected from one of sodium hypochlorite, potassium hypochlorite, calcium hypochlorite, sodium hypobromite, potassium hypobromite, and calcium hypobromite, preferably sodium hypochlorite or calcium hypochlorite.

[0026] As a preferred embodiment, without compromising the effects of the present invention, in order to smoothly proceed with the halogenation reaction, in the F halogenation step, an interfacial compatibilizer may be added to the hypohalite aqueous solution in an amount of 0.5-10% by mass of the hypohalite aqueous solution, preferably 1-5%.

[0027] The interfacial compatibilizer is a physical and chemical compatibility generated between a solid and a liquid when the solid and the liquid contact to form an interface, and includes methanol, ethanol, propanol, isopropanol, butanol, phenol, ethyl acetate, tetrahydrofuran, methyl ethyl ketone, etc., selected from one or a mixture of two or more thereof, preferably ethanol and propanol.

[0028] The second object of the present invention is to provide skin-friendly textiles with antibacterial function. To achieve the above object, the present invention applies any of the above methods to prepare skin-friendly textiles with antibacterial function.

[0029] Specifically, the textiles with antibacterial function include hats, work clothes, clothing, underwear, socks, incontinence products, diapers, towels, bedding, sheets, mattresses, sofa covers, tablecloths, dry wipes, wet wipes, quilt covers, sportswear, gloves, cushions, rags, underwear, down jackets, cotton jackets, cotton quilts and other manufactured products.

[0030] In the method for preparing textiles with antimicrobial and skin-friendly properties, the precursor of the antimicrobial agent is the diallylamine structural unit in the copolymer. However, since diallylamine polymerization undergoes free radical chain growth reactions and also undergoes free radical chain transfer reactions, it cannot form long-chain polymers with larger molecular weights. To obtain polymers with higher molecular weights, copolymerization with other monomers is typically employed to reduce the occurrence of chain transfer reactions. To obtain a copolymer primarily composed of diallylamine structural units, the present invention employs the addition of a second monomer to the copolymer. To enhance the skin-friendliness of the fabric, the second monomer is preferably a nitrogen- or nitrogen-dialkylacrylamide derivative with good hydrophilicity, thereby achieving a more optimized process. The use of ethanol as the medium further facilitates the post-antimicrobial finishing of undegreased fabrics with a certain degree of water resistance.

[0031] The raw materials selected by the present invention are cheap and easily available, and the production cost is low. The halamine compound is coated on the surface of the textile fiber by radiation, and then the textile is prepared as a textile with antibacterial function. The fiber fabric is used as a textile and also serves as a carrier support for antibacterial functional compounds such as antibacterial and sterilizing compounds. When people use the textile to achieve antibacterial purposes such as antibacterial and sterilizing, the antibacterial agent will not be scattered into the environment in the form of small molecules to cause secondary pollution to the environment, thereby achieving a safe and environmentally friendly antibacterial purpose.

[0032] The antibacterial textiles of the present invention can be applied to various manufactured products such as hats, work clothes, clothing, underwear, socks, incontinence products, diapers, towels, bedding, sheets, mattresses, sofa covers, tablecloths, dry wipes, wet wipes, quilt covers, sportswear, gloves, cushions, rags, underwear, down jackets, cotton-padded jackets, and cotton wadding. DETAILED DESCRIPTION

[0033] The present invention is further illustrated by the following examples, which, however, are not intended to limit the scope of the present invention.

[0034] Example 1

[0035] This example is a method for preparing a skin-friendly fabric with antibacterial function, which includes the following steps:

[0036] A. Preparation of impregnation solution:

[0037] In a stirring device 1.0m 3 In a mixer, add 200 kg of ethanol, 10 kg of diallylamine, 0.5 kg of N,N-dimethylacrylamide, 8.0 kg of N,N-diethylacrylamide, and 1.5 kg of methylenebisacrylamide in sequence, stir for 5 to 10 minutes to mix evenly, and finally adjust the amount of ethanol to prepare an impregnation solution with a comonomer mass concentration of 8.5%.

[0038] B. Impregnation finishing:

[0039] The nylon fabric was pre-soaked in ethanol and then placed in a deliquescence machine for deliquescence. The measured residual rate was 30%. Based on the absorption of 0.8% of the absolute dry mass of the comonomer, the concentration of the impregnation solution should be adjusted to 2.67%.

[0040] The above impregnation liquid is added to the impregnation tank, and ethanol is added to adjust the comonomer concentration of the impregnation liquid to 2.67%. Then the nylon fabric is placed in the impregnation tank and allowed to soak in the impregnation liquid for 3 to 5 minutes, and then moved into the deliquoring machine to remove the impregnation liquid to obtain the impregnated polypropylene fabric.

[0041] C. Drying:

[0042] Then, the impregnated nylon fabric which has been impregnated and finished is placed in a drying room with an ethanol recovery device at 50-55° C. to dry and remove the ethanol to obtain the dried nylon fabric.

[0043] The drying and removing of ethanol is carried out in a drying room at 30-80°C, preferably 30-50°C to remove the ethanol.

[0044] The drying room is a heating device with ethanol recovery function and capable of providing heat, including an oven, a drum dryer, a tunnel heating furnace, etc., and is selected from one or a mixture of two or more of them, preferably a tunnel heating furnace.

[0045] D. Irradiation:

[0046] Then, the dried nylon fabric was placed in a 40 cm*40 cm pressure-resistant plastic bag with sealing function, vacuumed, and then injected with 0.015 MPa industrial nitrogen. This was repeated three times and then sealed. After being flattened, the bag was placed on the conveyor belt of a 5 MeV high-energy electron beam accelerator irradiation device and irradiated at a dose of 48 kGy to obtain irradiated nylon fabric.

[0047] Specifically, the electron beam accelerator is a high-energy electron beam accelerator, including a high-voltage accelerator, an induction accelerator, and a resonant accelerator.

[0048] E. Extraction:

[0049] Then, fill the irradiated polypropylene fabric with 0.5m 3 The extraction kettle was filled with 25 kg of ethanol, which was then sealed and filled with liquid CO2. The process was adjusted to perform extraction at a supercritical temperature of 45°C and 8.0 MPa to dissolve the unreacted monomers. After 45 minutes of extraction, the pressure was removed, and the unreacted residual monomers were separated and removed to obtain the extracted nylon fabric.

[0050] The entrainer is a solvent with good compatibility with the residual monomers, including ethanol, methanol, etc., selected from one or a mixture of two thereof, preferably ethanol. The amount of the entrainer is 5.0-40.0% of the mass fraction of CO2.

[0051] The supercritical extraction device is a device that uses supercritical fluid extraction technology to perform extraction operations, and realizes the extraction and separation of residual unpolymerized monomers from irradiated solid fibers. The main equipment in the process is composed of a high-pressure extraction kettle, a separation kettle, a heat exchanger, a high-pressure pump (compressor), a storage tank, and pipes, valves and joints connecting these devices. The extraction time is 0.5 to 1.0 hours.

[0052] F. Halogenation:

[0053] After adjusting the pH value of the calcium hypochlorite aqueous solution to 6.8-7.5 with dilute hydrochloric acid, the mass percentage concentration of the calcium hypochlorite is adjusted to 1.5% with water, and then ethanol is added and mixed evenly to obtain a halogenated liquid, wherein the amount of ethanol added is 1.0% of the mass of the calcium hypochlorite aqueous solution.

[0054] Finally, the extracted nylon fabric is immersed in the halogenation solution and subjected to a halogenation reaction at room temperature for 60 minutes. The fabric is then taken out for dehydration and dried at 45-50° C. to obtain a textile having antibacterial and skin-friendly properties coated with an N-halogenated diallylamine copolymer having the structure represented by general formula (I).

[0055]

[0056] In formula (I), X represents a halogen atom such as chlorine or bromine, preferably a chlorine atom; and n represents the degree of polymerization.

[0057] Obtain nylon fabric with antibacterial function.

[0058] Example 2

[0059] This example is a method for preparing a skin-friendly fabric with antibacterial function, which includes the following steps:

[0060] A. Preparation of impregnation solution:

[0061] In a stirring device 1.0m 3 In a mixer, 200 kg of ethanol, 9.5 kg of diallylamine, 8.5 kg of N,N-dimethylacrylamide, and 2.0 kg of methylenebisacrylamide were added in sequence, and stirred for 5 to 10 minutes to mix evenly. Finally, the amount of ethanol was adjusted to prepare an impregnation solution with a comonomer mass concentration of 8.0%.

[0062] B. Impregnation finishing:

[0063] The polyester woven fabric was pre-soaked in ethanol and then placed in a de-liquidator for de-liquidation. The measured residual rate was 32%. Based on 1.0% of the absolute dry mass of the absorbed comonomer, the concentration of the impregnation solution should be adjusted to 3.13%.

[0064] The impregnation liquid is added to an impregnation tank, and ethanol is added to adjust the comonomer concentration of the impregnation liquid to 3.13%. The polyester woven fabric is then placed in the impregnation tank and allowed to soak in the impregnation liquid for 3 to 6 minutes. The impregnation liquid is then removed from the impregnation tank to obtain the impregnated polyester woven fabric.

[0065] C. Drying:

[0066] Then the impregnated polyester woven fabric which has been impregnated and finished is placed in a drying room with an ethanol recovery device at 55-60° C. to dry and remove the ethanol to obtain the dried polyester woven fabric.

[0067] D. Irradiation:

[0068] Next, the dried polyester woven fabrics were divided into 40 cm x 45 cm pressure-resistant plastic bags with sealing functions. The bags were vacuumed and then filled with 0.018 MPa industrial nitrogen three times before being sealed. The bags were flattened and placed on the conveyor belt of a 5 MeV high-energy electron beam accelerator irradiation device. They were irradiated at a dose of 52 kGy to produce irradiated polyester woven fabrics.

[0069] E. Extraction:

[0070] Then, fill the irradiated polyester woven fabric with 0.5M3 The extraction kettle was filled with 28 kg of ethanol, which was then sealed and filled with liquid CO2. The process was adjusted to extract under a supercritical state of 40 ° C and 7.8 MPa to dissolve the unreacted monomers. After extraction for 55 minutes, the pressure was unloaded, and the unreacted residual monomers were separated and removed to obtain extracted polyester woven fabric.

[0071] F. Halogenation:

[0072] After adjusting the pH value of the sodium hypochlorite aqueous solution to 7.0-7.5 with dilute hydrochloric acid, the mass percentage concentration of the sodium hypochlorite is adjusted to 2.0% with water, and then ethanol is added and mixed uniformly to obtain a halogenated liquid, wherein the amount of ethanol added is 1.2% of the mass of the sodium hypochlorite aqueous solution.

[0073] Finally, the extracted polyester woven fabric was immersed in the halogenation solution and subjected to halogenation reaction at room temperature for 60 minutes. The fabric was then taken out for dehydration and dried at 45-50° C. to obtain the antibacterial and skin-friendly polyester woven fabric.

[0074] Example 3

[0075] This example is a method for preparing an antibacterial fabric, which includes the following steps:

[0076] A. Preparation of impregnation solution:

[0077] In a stirring device 1.0M 3 In a mixer, 200 kg of ethanol, 10.5 kg of diallylamine, 1.5 kg of N,N-diethylacrylamide, 6.2 kg of N,N-dimethylacrylamide, and 1.8 kg of methylenebisacrylamide were added in sequence, and stirred for 5 to 10 minutes to mix evenly. Finally, the amount of ethanol was adjusted to prepare an impregnation solution with a comonomer mass concentration of 8.0%.

[0078] B. Impregnation finishing:

[0079] The polyester-cotton fabric blended with 35% cotton and 65% polyester was soaked in ethanol in advance and then placed in a deliquoring machine for deliquoring. The measured residual rate was 36%. Based on the absorption of 0.75% of the absolute dry mass of the comonomer, the concentration of the impregnation solution should be adjusted to 2.08%.

[0080] The above impregnation liquid is added to the impregnation tank, and ethanol is added to adjust the comonomer concentration of the impregnation liquid to 2.08%. Then the polyester-cotton fabric is placed in the impregnation tank and allowed to soak in the impregnation liquid for 3 to 6 minutes. It is then moved into the de-liquidator to remove the impregnation liquid to obtain the impregnated polyester-cotton fabric.

[0081] C. Drying:

[0082] Then, the impregnated polyester-cotton fabric after impregnation and finishing is placed in a drying room with an ethanol recovery device at 45-50° C. to dry and remove the ethanol to obtain a dried polyester-cotton fabric.

[0083] D. Irradiation:

[0084] Next, the dried polyester-cotton fabrics were divided into 45 cm*45 cm pressure-resistant plastic bags with sealing function, vacuumed, and then injected with 0.016 MPa industrial nitrogen. This process was repeated three times and then sealed. After being flattened, the bags were placed on the conveyor belt of a 5 MeV high-energy electron beam accelerator irradiation device and irradiated at a dose of 42 kGy to obtain irradiated polyester-cotton fabrics.

[0085] E. Extraction:

[0086] Then, fill the irradiated polyester-cotton fabric with 0.5M 3 The extraction kettle was filled with 30 kg of ethanol, which was then sealed and filled with liquid CO2. The process was adjusted to perform extraction under a supercritical state of 42°C and 7.8 MPa to dissolve the unreacted monomers. After 50 minutes of extraction, the pressure was unloaded, and the unreacted residual monomers were separated and removed to obtain the extracted polyester-cotton fabric.

[0087] F. Halogenation:

[0088] After adjusting the pH value of the sodium hypochlorite aqueous solution to 6.7-7.2 with nitric acid and hydrochloric acid, the mass percentage concentration of the sodium hypochlorite is adjusted to 2.5% with water, and then ethanol is added and mixed evenly to obtain a halogenated liquid, wherein the amount of ethanol added is 1.5% of the mass of the sodium hypochlorite aqueous solution.

[0089] Finally, the extracted polyester-cotton fabric is immersed in the halogenation solution and subjected to halogenation reaction at room temperature for 60 minutes. The fabric is then taken out for dehydration and dried at 45-50° C. to obtain a polyester-cotton fabric with antibacterial and skin-friendly properties.

[0090] Example 4

[0091] This example is a method for preparing an antibacterial fabric, which includes the following steps:

[0092] A. Preparation of impregnation solution:

[0093] In a stirring device 1.0M 3 In a mixer, add 200 kg of ethanol, 9 kg of diallylamine, 9.0 kg of N,N-diethylacrylamide, 1.0 kg of N,N-dimethylacrylamide, and 1.0 kg of methylenebisacrylamide in sequence, stir for 5 to 10 minutes to mix evenly, and finally adjust the amount of ethanol to prepare an impregnation solution with a comonomer mass concentration of 8.5%.

[0094] B. Impregnation finishing:

[0095] The vinylon-cotton blended fabric was pre-soaked in ethanol and then placed in a deliquoring machine for deliquoring. The residual rate was measured to be 46%. Based on the absorption of 1.1% of the absolute dry mass of the comonomer, the concentration of the impregnation solution should be adjusted to 2.39%.

[0096] The above impregnation liquid is added into the impregnation tank, and ethanol is added to adjust the comonomer concentration of the impregnation liquid to 2.39%. Then the cotton fabric is placed into the impregnation tank and allowed to soak in the impregnation liquid for 3 to 5 minutes. Then the fabric is moved into the deliquoring machine to remove the impregnation liquid to obtain the impregnated cotton fabric.

[0097] C. Drying:

[0098] Then, the impregnated cotton fabric that has been impregnated and finished is placed in a drying room with an ethanol recovery device at 45-48° C. to dry and remove the ethanol to obtain the dried cotton fabric.

[0099] D. Irradiation:

[0100] Next, the dried cotton fabrics were divided into 42 cm*42 cm pressure-resistant plastic bags with sealing function, vacuumed, and then injected with 0.016 MPa industrial nitrogen. This process was repeated three times and then sealed. After being flattened, the bags were placed on the conveyor belt of a 5 MeV high-energy electron beam accelerator irradiation device and irradiated at a dose of 52 kGy to obtain irradiated cotton fabrics.

[0101] E. Extraction:

[0102] Then, fill the irradiated cotton fabric with 0.5M 3 The extraction kettle was added with 25 kg of ethanol, which was then sealed and filled with liquid CO2. The process was adjusted to perform extraction at a supercritical state of 45 ° C and 7.7 MPa to dissolve the unreacted monomers. After 45 minutes of extraction, the pressure was unloaded, and the unreacted residual monomers were separated and removed to obtain the extracted fiber-cotton fabric.

[0103] F. Halogenation:

[0104] After adjusting the pH value of the calcium hypochlorite aqueous solution to 6.8-7.5 with dilute hydrochloric acid, the mass percentage concentration of the calcium hypochlorite is adjusted to 1.75% with water, and then ethanol is added and mixed evenly to obtain a halogenated liquid, wherein the amount of ethanol added is 1.25% of the mass of the calcium hypochlorite aqueous solution.

[0105] Finally, the extracted cotton fabric was immersed in the halogenation solution and subjected to halogenation reaction at room temperature for 65 minutes. The fabric was then taken out for dehydration and dried at 45-50° C. to obtain a cotton fabric with antibacterial and skin-friendly properties.

[0106] Example 5

[0107] This example is a method for preparing an antibacterial fabric, which includes the following steps:

[0108] A. Preparation of impregnation solution:

[0109] In a stirring device 1.0M 3 In a mixer, 200 kg of ethanol, 11 kg of diallylamine, 0.8 kg of N,N-diethylacrylamide, 6.4 kg of N,N-dimethylacrylamide, and 1.8 kg of methylenebisacrylamide were added in sequence, and stirred for 5 to 10 minutes to mix evenly. Finally, the amount of ethanol was adjusted to prepare an impregnation solution with a comonomer mass concentration of 9.0%.

[0110] B. Impregnation finishing:

[0111] The nylon cotton was soaked in ethanol in advance and then placed in a deliquoring machine for deliquoring. The residual rate was measured to be 38%. Based on the absorption of 0.8% of the absolute dry mass of the comonomer, the concentration of the impregnation liquid should be adjusted to 2.11%.

[0112] The above impregnation liquid is added into the impregnation tank, and ethanol is added to adjust the comonomer concentration of the impregnation liquid to 2.11%. Then the nylon cotton is put into the impregnation tank and allowed to soak in the impregnation liquid for 3 to 5 minutes. Then it is moved into the deliquoring machine to remove the impregnation liquid to obtain the impregnated nylon cotton.

[0113] C. Drying:

[0114] Then, the impregnated cotton that has been impregnated and finished is placed in a drying room with an ethanol recovery device at 45-50° C. to dry and remove the ethanol to obtain dried cotton.

[0115] D. Irradiation:

[0116] Next, the dried cotton was divided into 40cm*40cm pressure-resistant plastic bags with sealing function, vacuumed, and then injected with 0.015MPa industrial nitrogen. This was repeated three times and then sealed. After being flattened, the bags were placed on the conveyor belt of a 5Mev high-energy electron beam accelerator irradiation device and irradiated at a dose of 45kGy to obtain irradiated cotton.

[0117] E. Extraction:

[0118] Then, fill the irradiated cotton with 0.5M 3 The extraction kettle was filled with 25 kg of ethanol, which was then sealed and filled with liquid CO2. The process was adjusted to extract at 45 ° C and 8.0 MPa supercritical state to dissolve the unreacted monomers. After 50 minutes of extraction, the pressure was unloaded, and the unreacted residual monomers were separated and removed to obtain extracted cotton.

[0119] F. Halogenation:

[0120] After adjusting the pH value of the calcium hypochlorite aqueous solution to 6.8-7.3 with dilute hydrochloric acid, the mass percentage concentration of the calcium hypochlorite is adjusted to 3.0% with water, and then ethanol is added and mixed uniformly to obtain a halogenated liquid, wherein the amount of ethanol added is 2.0% of the mass of the calcium hypochlorite aqueous solution.

[0121] Finally, the extracted cotton was immersed in the halogenation solution, and the halogenation reaction was carried out at room temperature for 60 minutes. Then, the cotton was taken out for dehydration and dried at 45-50°C to obtain cotton with antibacterial and skin-friendly functions.

[0122] Example 6

[0123] This example is a method for preparing mountaineering clothing with antibacterial function.

[0124] In this example, the antibacterial nylon fabric prepared in Example 1 is used to make mountaineering clothes with antibacterial function.

[0125] Example 7

[0126] This example is a method for preparing work clothes with antibacterial function.

[0127] In this example, the antibacterial polyester woven fabric prepared in Example 2 is used to make work clothes with antibacterial function.

[0128] Example 8

[0129] This example is a method for preparing a shirt with antibacterial function.

[0130] In this example, the antibacterial polyester-cotton fabric prepared in Example 3 is used to make a shirt with antibacterial function.

[0131] Example 9

[0132] This example is a method for preparing underwear with antibacterial function.

[0133] In this example, the antibacterial cotton fabric prepared in Example 4 is used as the skin-contacting layer to make underwear with antibacterial function.

[0134] Example 10

[0135] This example is a method for preparing cotton clothing with antibacterial function.

[0136] In this example, the antibacterial cotton prepared in Example 5 is used to make cotton clothing with antibacterial function.

Claims

1. A method for preparing skin-friendly textiles with antibacterial function, characterized in that The following steps are involved: A. Preparation of impregnation solution: In a reactor, ethanol, diallylamine, and a second monomer are sequentially added and stirred and mixed. The amount of ethanol is adjusted to prepare a solution with a comonomer concentration of 5.0 to 10.0%. The mixture is stirred and mixed until uniformly distributed to obtain an impregnation solution. The amount of diallylamine added is 30.0 to 60.0% of the mass fraction of the comonomer. The second monomer is N,N-diethylacrylamide or N,N-dimethylacrylamide, or a mixture of the two. B. Impregnation finishing: Then, the impregnation liquid is used to impregnate the textile using an impregnation and de-impregnation device to obtain an impregnated textile, with a rolling rate of 20 to 120%. The concentration of the impregnation liquid is adjusted to 0.01 to 3.0% of the absolute dry weight of the comonomer absorbed by the textile; C. Drying: drying the impregnated textile after impregnation treatment to remove ethanol to obtain a dried textile; D. Irradiation: Then, the dried textiles are irradiated in a controlled atmosphere to obtain irradiated textiles; E. Extraction: The irradiated textile and the entrainer are then placed together in an extraction kettle of a supercritical extraction device, and unreacted monomers are dissolved by extraction with CO2 in a supercritical state, and then separated in a separation kettle to remove unreacted residual monomers to obtain an extracted textile. The entrainer is a solvent that has good solubility in the residual monomers, selected from ethanol, methanol, or a mixture of the two. The amount of the entrainer is 5.0 to 40.0% of the mass fraction of the CO2. F. Halogenation: The extracted textile subjected to the extraction treatment is immersed in an aqueous hypohalite solution having a pH value of 6.5 to 7.5 and a mass percentage concentration of 0.1 to 10.0%, and a halogenation reaction is carried out at room temperature for 30 to 80 minutes. The textile is then taken out for dehydration and dried at a temperature of 40 to 50° C. to obtain a skin-friendly textile having an antibacterial function and coated with an N-halodiallylamine copolymer having a structure represented by general formula (I); In formula (I), X represents a halogen atom such as chlorine or bromine; and n represents the degree of polymerization.

2. The preparation method according to claim 1, wherein: In the preparation of the impregnation solution in step A, diallylamine and the second monomer are sequentially added to the reactor, and then a crosslinking agent monomer is added in an amount of 0.01 to 30.0% of the mass fraction of the comonomer.

3. The preparation method according to claim 2, wherein: The crosslinking agent monomer is selected from one or a mixture of two or more of diisopropenylbenzene, divinylbenzene, triallylamine, methylenebisacrylamide, ethylene glycol diacrylate, ethylene glycol dimethacrylate, diethylene glycol diacrylate, triethylene glycol diacrylate, 1,4-butanediol diacrylate, trimethylolpropane triacrylate, and pentaerythritol triacrylate.

4. The preparation method according to claim 1, wherein: The irradiation treatment refers to irradiating the dried textiles with an electron beam accelerator at a dose of 10 to 150 kGy.

5. The preparation method according to claim 4, characterized in that: The electron beam accelerator is a high-energy electron beam accelerator.

6. A skin-friendly textile with antibacterial function produced by the method according to any one of claims 1 to 5.

Citation Information

Patent Citations

  • Antimicrobial treating agent

    JP1995187936A