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WO2021232870A1 - 一种含铜抗菌、抗病毒无纺布及其制备方法 - Google Patents

一种含铜抗菌、抗病毒无纺布及其制备方法 Download PDF

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Publication number
WO2021232870A1
WO2021232870A1 PCT/CN2021/077409 CN2021077409W WO2021232870A1 WO 2021232870 A1 WO2021232870 A1 WO 2021232870A1 CN 2021077409 W CN2021077409 W CN 2021077409W WO 2021232870 A1 WO2021232870 A1 WO 2021232870A1
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WO
WIPO (PCT)
Prior art keywords
copper
fiber
spunlace
woven fabric
solution
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/CN2021/077409
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English (en)
French (fr)
Inventor
许东东
许心愿
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Harvest Spf Textile Beijing Co Ltd
Original Assignee
Harvest Spf Textile Beijing Co Ltd
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Filing date
Publication date
Application filed by Harvest Spf Textile Beijing Co Ltd filed Critical Harvest Spf Textile Beijing Co Ltd
Publication of WO2021232870A1 publication Critical patent/WO2021232870A1/zh
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • D—TEXTILES; PAPER
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    • D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
    • D06M2101/28—Acrylonitrile; Methacrylonitrile
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/32—Polyesters
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/16—Synthetic fibres, other than mineral fibres
    • D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M2101/34—Polyamides
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2201/00—Cellulose-based fibres, e.g. vegetable fibres
    • D10B2201/01—Natural vegetable fibres
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2321/00—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D10B2321/10—Fibres made from polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
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    • D10B2401/00—Physical properties
    • D10B2401/13—Physical properties anti-allergenic or anti-bacterial

Definitions

  • This application relates to the technical field of non-woven fabrics, and more specifically, it relates to a copper-containing antibacterial and antiviral non-woven fabric and a preparation method thereof.
  • Spunlace non-woven fabrics are fabrics in which high-pressure fine water jets are sprayed onto one or more layers of fiber webs to entangle the fibers so that the webs can be reinforced and have a certain strength. Because of its advantages of high strength, low fuzz, high moisture absorption and good air permeability, spunlace nonwovens have become one of the fastest technological advancements in the nonwovens industry in recent years, and are widely used in medical and sanitary nonwovens. Fabrics, non-woven fabrics for home decoration, non-woven fabrics for clothing, non-woven fabrics for industrial use, non-woven fabrics for agricultural use, etc. In particular, in recent years, while the demand for medical and health non-woven fabrics has greatly increased, higher requirements have been placed on its antibacterial and antiviral properties.
  • non-woven fabrics are conducive to the adhesion of microorganisms due to their porous shape and the chemical structure of polymer compounds. Therefore, the research and development of antibacterial functions of spunlace non-woven fabrics is of great significance.
  • this application provides a method for preparing copper-containing antibacterial and antiviral non-woven fabrics, which has good antibacterial properties and a certain degree of antiviral spunlace.
  • the woven fabric has the advantages of simple preparation method, easy realization of industrialization, and simple process.
  • this application provides the following technical solution: a method for preparing a copper-containing antibacterial and antiviral non-woven fabric, including the following steps:
  • the fiber material is successively subjected to fiber web formation, pre-wetting, and spunlace reinforcement to obtain a spunlace fiber fabric base fabric;
  • the spunlace fiber cloth base fabric is padding sizing in an organic complex copper solution to obtain a copper-containing spunlace non-woven fabric, and the copper content of the copper-containing spunlace non-woven fabric is ⁇ 500ppm;
  • the copper-containing spunlace non-woven fabric obtained after padding and sizing is dried and wound.
  • the copper element has a strong bactericidal function and a certain antiviral effect.
  • the spunlace non-woven fabric is padding sizing in the organic complex copper solution.
  • the organic complex copper solution Not only can be coated on the surface of the spunlace non-woven fabric, but also can penetrate into the internal voids of the spunlace non-woven fabric, making the interior of the spunlace non-woven fabric, especially the voids between the fibers and the surface of the spunlace non-woven fabric All have copper ions, which can play a better antibacterial effect.
  • the copper element exists in the form of copper ions between the fibers of the spunlace non-woven fabric, and the antibacterial function is more significant, especially the copper-containing spunlace
  • the control of the copper ion concentration on the non-woven fabric makes the final spunlace non-woven fabric have excellent antibacterial and antiviral effects.
  • the fibrous material fibers are first formed into a web, then pre-wet, and then reinforced by hydroentanglement. Under the action of hydroentanglement, the fiber web moves, intersperses, entangles, and entangles among the fibers. , Forming countless soft entanglement points, consolidating the fiber web to obtain the spunlace fiber cloth base fabric.
  • the pre-wetting operation compacts the fluffy fiber web, venting the air in the fiber web, so that the fiber web can enter the spunlace area.
  • the spunlace non-woven fabric in the present application is directly padding sizing after fiber formation and spunlace reinforcement during the production process.
  • the operation is more simple and convenient, and the process cycle is more convenient. Shorter, large-scale production of spunlace non-woven fabrics in a short period of time, to meet the supply, and can meet the performance of non-woven fabrics, and has excellent antibacterial and antiviral properties. It can be used in disposable medical supplies.
  • padding through the organic complex copper solution makes the gaps and areas of the spunlace non-woven fabric evenly infiltrated, and the antibacterial effect is uniform, which can effectively avoid Precipitation of substances in the holes of the spunlace non-woven fabric after drying.
  • the fiber material includes at least one of natural fiber, rayon fiber, rayon protein fiber, polyacrylonitrile fiber, and polyvinyl alcohol fiber.
  • the molecular structure of the fiber material contains open hydroxyl groups
  • the formed spunlace fiber cloth base cloth contains open hydroxyl groups.
  • the fabric obtained after the step of forming the fiber material fiber into the web contains ⁇ 5% cotton fiber, or 5-65% cellulose fiber, or 5-65% protein fiber, or 5-65% poly Acrylonitrile fiber, or 100% low melting point polyvinyl alcohol fiber;
  • the organic complex copper solution is obtained by adding 5.5 wt% of the initial organic complex copper solution to 10-30 volume multiples of water.
  • the fabric when the fabric is 100% low-melting point polyvinyl alcohol fiber, it can be dissolved in low-temperature water, which reduces waste generation, especially for the current medical waste treatment.
  • the initial organic complexed copper solution is prepared according to the following method:
  • Preparation of organic complex copper solution add the coordination solid mixture including sodium chloride, potassium permanganate, sodium peroxide and copper powder to the coordination ionic liquid, stir uniformly, react, and pour into pure water after cooling to obtain the copper content It is 5.5wt% of the initial organic copper complex solution.
  • the organic complex copper solution is used in the spunlace non-woven fabric in this application.
  • organic copper is safer and more reliable, has good environmental compatibility, and has good compatibility. Its antibacterial effect lasts for a long time, and the copper content on the final spunlace non-woven fabric can be controlled by the copper ion concentration in the initial organic complexed copper solution and the amount of water added, and finally has excellent antibacterial and antiviral properties.
  • the application is further set as follows: in the step of preparing the coordination ionic liquid, the mixing weight ratio of urea, caprolactam and acetamide is 1: (0.2-0.4): (0.2-0.4), and the heating temperature after uniform mixing is 100-120°C, The holding time is 0.5-1h.
  • the application is further set as follows: in the step of preparing the organic complex copper solution: the mixing weight ratio of sodium chloride, potassium permanganate, sodium peroxide and copper powder is 1: (1-2): (1-2): ( 2.5-2.9), the mixing weight ratio of the coordination solid mixture and the coordination ionic liquid is 1: (3-3.5).
  • the application is further configured as follows: when the fiber material is one or more of polyester fiber, polyamide fiber, polyvinyl chloride fiber, and polypropylene fiber, the spunlace fiber cloth base fabric is also shelled before padding and sizing.
  • the dipping step of the glycan-ascorbic acid solution is as follows: the spunlace fiber cloth base cloth is dipped in the chitosan-ascorbic acid solution, and then dried at 150-170°C for 5-10min, the chitosan-ascorbic acid solution
  • the preparation method is as follows: add 5-10 parts of chitosan powder to 25-30 parts of acetic acid and 60-70 parts of water, magnetically stir until the chitosan is dissolved, then add 3-5 parts of ascorbic acid, and stir evenly.
  • the molecular structures of chitosan and ascorbic acid both have open hydroxyl groups.
  • the spunlace fiber cloth base fabric is first dipped in a chitosan-ascorbic acid solution, and the chitosan and ascorbic acid are immersed in the spunlace fiber cloth.
  • the hydroxyl binding points on the reinforced spunlace fiber cloth base fabric will have more binding sites with the complex copper ions during the subsequent padding in the organic complex copper solution.
  • the coordination bond of monovalent copper is more covalent, so the stability of monovalent copper complexes is stronger than that of divalent copper complexes.
  • the strong ascorbic acid is used in this application. Reducing, adding ascorbic acid can inhibit the oxidation of monovalent copper to divalent copper, thereby enhancing the antibacterial performance and the durability of antibacterial functions.
  • Chitosan is also added to the system, and the dissolved chitosan has a strong adsorption capacity. Chitosan can be more firmly attached between the spunlace fiber cloth base cloth, and it can also improve the ascorbic acid and spunlace fiber cloth. The bonding strength between the base fabrics.
  • the addition of acetic acid can dissolve chitosan on the one hand, and on the other hand, it can also enhance the adsorption between chitosan and the spunlace fiber fabric, so that chitosan and ascorbic acid can be more firmly adsorbed on the spunlace fiber fabric. After drying, the chitosan also has certain antibacterial properties and excellent moisture absorption properties, which can further enhance the antibacterial and moisture absorption properties of the spunlace fiber cloth.
  • the application is further set as follows: the spunlace fiber cloth base cloth is subjected to a soaping step after the chitosan-ascorbic acid solution padding step, and the specific operation is: the dried spunlace fiber cloth base cloth is soaped at 5g/L Medium soaping 5-10min, soaping temperature is 35-40°C, and then drying at 50-60°C.
  • the spunlace fiber cloth base fabric after the chitosan-ascorbic acid solution is soaked can be soaped, which can remove the weakly bonded chitosan and ascorbic acid on the spunlace fiber cloth base fabric and prevent subsequent soaking.
  • chitosan and ascorbic acid enter the organic complexed copper solution and complex with complexed copper ions.
  • the present application provides a copper-containing antibacterial and antiviral non-woven fabric, which has the advantages of good antibacterial properties and certain antiviral properties.
  • this application provides the following technical solution: a copper-containing antibacterial and antiviral non-woven fabric prepared by the preparation method according to the first aspect described above.
  • the spunlace nonwoven fabric prepared by the above method has improved antibacterial and antiviral properties on the basis of maintaining excellent air permeability, high moisture absorption and low fluffing of the spunlace nonwoven fabric.
  • the obtained spunlace non-woven fabric has excellent antibacterial and antiviral properties, and has a wide range of applications.
  • this application provides an application of a copper-containing antibacterial and antiviral non-woven fabric, which has the advantage of being widely used.
  • this application provides the following technical solution: an application of the above-mentioned copper-containing antibacterial and antiviral non-woven fabric in medical and sanitary products.
  • the non-woven fabric obtained in this application has excellent antibacterial and disease resistance performance, and has a wide range of products in medical and sanitary products such as surgical gowns, surgical masks, medical dressing materials, wound dressings, medical gauze, and masks. Applications.
  • the spunlace non-woven fabric is padding sizing in the organic complex copper solution.
  • the copper element is present in the spunlace in the form of complexed copper ions.
  • the antibacterial function between the fibers of the woven fabric is more significant, especially by controlling the concentration of copper ions on the spunlace non-woven fabric, which has an antibacterial and antiviral effect.
  • the organic complex copper solution can not only be coated on the spunlace
  • the surface of the non-woven fabric can penetrate into the internal voids of the spunlace non-woven fabric, so that the interior of the spunlace non-woven fabric, especially the voids between the fibers and the surface of the spunlace non-woven fabric, have copper ions, which can Play a better antibacterial effect;
  • the spunlace non-woven fabric in the present application is directly padding sizing after fiber formation and spunlace reinforcement during the production process.
  • the padding makes the gaps and areas of the spunlace non-woven fabric evenly infiltrated, and the antibacterial effect is uniform, which can effectively avoid the precipitation of substances in the spunlace non-woven fabric holes after drying; on the other hand, the operation is more simple and convenient.
  • the process cycle is shorter, and the spunlace non-woven fabric can be mass-produced in a short time to meet the supply, and can meet the performance of the non-woven fabric, and has excellent antibacterial and antiviral properties. It can be used in disposable medical products. The demand and supply of various medical supplies during the epidemic is of great significance;
  • the fiber material used for fiber web formation in this application includes at least one of natural fiber, rayon fiber, rayon fiber, polyacrylonitrile fiber, and polyvinyl alcohol fiber, so that the spunlace fiber cloth base fabric contains The open hydroxyl group will form a chemical chelation between the copper complex and the hydroxyl group during subsequent padding in the organic complex copper solution. The two are firmly combined and will not easily fall off during use. The resulting spunlace fiber cloth is antibacterial and durable. Excellent performance.
  • the spunlace process can process various fibers, such as cotton fiber, nylon fiber, polypropylene fiber, polyester fiber or viscose fiber and other common fibers. Therefore, in the preparation step of the spunlace non-woven fabric base fabric in this application
  • the material of the obtained spunlace non-woven fabric is not limited.
  • cellulose fiber such as viscose fiber, etc.
  • protein fiber such as peanut protein fiber, etc.
  • polyester fiber polyamide fiber ( Nylon/nylon), polyacrylonitrile fiber (acrylic), polyvinyl chloride fiber (chlorinated fiber), polypropylene fiber (polypropylene) or polyvinyl alcohol fiber (Villen), control water by controlling the copper content in the organic complex copper solution
  • the content of copper on the barbed fiber cloth is ⁇ 500 ppm, more preferably 1000-8000 ppm.
  • the fiber material used for fiber formation includes any one of natural fibers or fibers obtained by wet spinning. Specifically, it includes natural fibers such as cotton fibers, man-made cellulose fibers, and man-made fibers. At least one of protein fiber, polyacrylonitrile fiber, and polyvinyl alcohol fiber.
  • the above-mentioned fibers all contain hydroxyl groups, and the fabrics obtained after forming the net on the netting curtain contain open hydroxyl groups, which can form chemical chelation with the complex copper ions when they are paddled in the organic complex copper solution.
  • the combination is more tight, such as the fiber material is only viscose fiber or peanut protein fiber, or a mixture of viscose fiber and peanut protein fiber.
  • the fabric obtained after the fiber material fiber web-forming step contains ⁇ 5wt% cotton fiber, or 5-65wt% cellulose fiber, or 5-65wt% protein fiber, or 5-65wt% polyacrylonitrile
  • the fiber, or 100% low-temperature water-soluble polyvinyl alcohol fiber can use any one of the above-mentioned solutions, but is not limited to the above-mentioned solution.
  • the fiber material is a mixed fiber material of the above-mentioned hydroxyl-containing fibers and non-hydroxyl-containing fibers, the sum of the hydroxyl-containing fibers in the fabric after the fiber is formed into the web can reach the corresponding minimum content, such as cotton fiber and viscose fiber.
  • the low-temperature water-soluble polyvinyl alcohol fiber can be directly dissolved in low-temperature water, and can be dissolved in water at 20-98°C.
  • the fiber material used for fiber formation such as the fiber material contains one or more of polyester fiber, polyamide fiber, polyvinyl chloride fiber, and polypropylene fiber, in order to improve the complex copper
  • the chitosan-ascorbic acid solution padding step is also carried out before padding and sizing. Both chitosan and ascorbic acid contain open hydroxyl groups, and then the chitosan is used.
  • the adsorption performance and the addition of acetic acid in the chitosan-ascorbic acid solution make the chitosan and ascorbic acid more firmly adhere to the spunlace fiber cloth base cloth, and complex copper ions in the organic complex copper solution to form chemical chelation to enhance the organic Bond strength between copper and spunlace fiber cloth.
  • Preparation examples 1-5 are preparation examples of the organic complex copper solution.
  • a preparation method of organic complex copper solution including the following steps:
  • a preparation method of organic complex copper solution including the following steps:
  • a preparation method of organic complex copper solution including the following steps:
  • a preparation method of the organic complex copper solution is carried out according to the method in Preparation Example 2, except that the initial organic complex copper solution is poured into 15 volume multiples of pure water to prepare the organic complex copper solution.
  • a preparation method of the organic complex copper solution is carried out according to the method in Preparation Example 2, except that the initial organic complex copper solution is poured into 25 volume multiples of pure water to prepare the organic complex copper solution.
  • Preparation examples 6-10 are preparation examples of chitosan-ascorbic acid solution.
  • a preparation method of chitosan-ascorbic acid solution includes the following steps:
  • a preparation method of chitosan-ascorbic acid solution includes the following steps:
  • a preparation method of chitosan-ascorbic acid solution includes the following steps:
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
  • spunlace non-woven fabric base fabric the mixed fiber material of viscose fiber and polyester fiber is sequentially subjected to fiber web formation, pre-wetting, and spunlace reinforcement to obtain a spunlace fiber fabric base fabric.
  • the fabric after fiber formation contains 5wt. % Of viscose fiber;
  • the spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution by a sizing machine to obtain a copper-containing spunlace non-woven fabric.
  • the organic complex copper solution in the sizing machine is prepared in Preparation Example 2 The organic complex copper solution;
  • the copper-containing spunlace non-woven fabric obtained after padding and sizing is dried and wound at a drying temperature of 90°C.
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
  • Spunlace non-woven fabric base fabric preparation the viscose fiber, polyacrylonitrile fiber and polyester fiber mixed fiber are sequentially fabricated, pre-wet, and spunlaced to obtain a spunlace fiber fabric base fabric.
  • the sum of viscose fiber and polyester fiber in the cloth is 65wt%;
  • the spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution by a sizing machine to obtain a copper-containing spunlace non-woven fabric.
  • the organic complex copper solution in the sizing machine is prepared in Preparation Example 1 The organic complex copper solution;
  • the copper-containing spunlace nonwoven fabric obtained after padding and sizing is dried and wound at a drying temperature of 100°C.
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
  • Spunlace non-woven fabric base fabric preparation Spunlace fiber fabric base fabric is obtained by combining cotton fiber and polyester fiber mixed fiber through fiber web formation, pre-wetting, and spunlace reinforcement.
  • the cotton fiber content in the fabric after fiber web formation is 5wt%;
  • the spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution through a sizing machine to obtain a copper-containing spunlace non-woven fabric.
  • the organic complex copper solution in the sizing machine is prepared in Preparation Example 5 The organic complex copper solution;
  • the copper-containing spunlace nonwoven fabric obtained after padding and sizing is dried and wound at a drying temperature of 100°C.
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics is carried out according to the method in Example 2, except that:
  • the soybean fiber and polyester fiber mixed fiber are sequentially subjected to fiber formation, pre-wetting, and spunlace reinforcement to obtain the spunlace fiber fabric base fabric.
  • the content of soybean fiber in the fabric after the fiber formation is 20wt%;
  • the organic complex copper solution in the sizing machine is the organic complex copper solution prepared in Preparation Example 3.
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics is carried out according to the method in Example 2, except that:
  • the low-temperature water-soluble polyvinyl alcohol fiber is successively subjected to fiber web formation, pre-wetting, and spunlace reinforcement to obtain the spunlace fiber fabric base fabric.
  • the low-temperature water-soluble polyvinyl alcohol can be Dissolve in the water temperature
  • the organic complex copper solution in the sizing machine is selected from the organic complex copper solution prepared in Preparation Example 4.
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
  • Spunlace fiber fabric base fabric is obtained after the polypropylene fiber is formed into a web, pre-wet, and spunlace reinforced in sequence;
  • Chitosan-ascorbic acid solution padding In the sizing machine, the spunlace fiber cloth is padding in the chitosan-ascorbic acid solution, and then dried at 150°C for 10 minutes. The chitosan-ascorbic acid solution in the sizing machine is selected The chitosan-ascorbic acid solution prepared in Preparation Example 6;
  • the dried spunlace fiber cloth base cloth is soaped in 5g/L soaping agent for 10 minutes, the soaping temperature is 35°C, and then dried at 50°C.
  • the soaping agent is purchased from Dongguan Spinning Chain New Material Technology Co., Ltd., the brand is Texchain, the model is 605;
  • the soaped spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution through the sizing machine to obtain the copper-containing spunlace non-woven fabric.
  • the preparation example of the organic complex copper solution in the sizing machine The organic complex copper solution prepared in 1;
  • the copper-containing spunlace nonwoven fabric obtained after padding and sizing is dried and wound at a drying temperature of 100°C.
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
  • the polyamide fiber is successively subjected to fiber formation, pre-wetting, and spunlace reinforcement to obtain the spunlace fiber fabric base fabric;
  • Chitosan-ascorbic acid solution padding In the sizing machine, the spunlace fiber cloth is padding in the chitosan-ascorbic acid solution, and then dried at 160°C for 8 minutes. The chitosan-ascorbic acid solution in the sizing machine is selected The chitosan-ascorbic acid solution prepared in Preparation Example 7;
  • the dried spunlace fiber cloth base fabric is soaped in 5g/L soaping agent for 5 minutes, the soaping temperature is 40°C, and then dried at 55°C.
  • the soaping agent is purchased from Dongguan Spinning Chain New Material Technology Co., Ltd., the brand is Texchain, the model is 605;
  • the soaped spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution through the sizing machine to obtain the copper-containing spunlace non-woven fabric.
  • the preparation example of the organic complex copper solution in the sizing machine The organic complex copper solution prepared in 2;
  • the copper-containing spunlace nonwoven fabric obtained after padding and sizing is dried and wound at a drying temperature of 100°C.
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
  • the polyvinyl chloride fiber is successively subjected to fiber web formation, pre-wetting, and spunlace reinforcement to obtain the spunlace fiber fabric base fabric;
  • Chitosan-ascorbic acid solution padding In the sizing machine, the spunlace fiber cloth base cloth is padding in the chitosan-ascorbic acid solution, and then dried at 170°C for 5 minutes. The chitosan-ascorbic acid solution in the sizing machine is selected The chitosan-ascorbic acid solution prepared in Preparation Example 8;
  • the dried spunlace fiber cloth base cloth is soaped in 5g/L soaping agent for 5 minutes, the soaping temperature is 40 °C, and then dried at 60 °C, of which, the soaping agent is purchased from Dongguan Spinning Chain New Material Technology Co., Ltd., the brand is Texchain, the model is 605;
  • the soaped spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution through the sizing machine to obtain the copper-containing spunlace non-woven fabric.
  • the preparation example of the organic complex copper solution in the sizing machine The organic complex copper solution prepared in 3;
  • the copper-containing spunlace nonwoven fabric obtained after padding and sizing is dried and wound at a drying temperature of 100°C.
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics is carried out according to the method in Example 2. The difference is that in the padding sizing step, when the organic complex copper solution in the sizing machine is prepared, the initial organic The copper complex solution was poured into pure water of 12 volume multiples, and the rest was the same as in Preparation Example 2.
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics is carried out according to the method in Example 2. The difference is that in the padding sizing step, when the organic complex copper solution in the sizing machine is prepared, the initial organic The copper complex solution was poured into pure water of 25 volume multiples, and the rest was the same as in Preparation Example 2.
  • a method for preparing copper-containing antibacterial and antiviral non-woven fabrics is carried out according to the method in Example 2. The difference is that in the padding sizing step, the solution in the sizing machine is not an organic complex copper solution, but 3mol/ L of copper chloride solution.
  • test sample is a disc with a diameter of 4.8 cm. 4 parallel tests are performed, and the average value is taken.
  • the tested strain is Methicillin-resistant Staphylococcus aureus ATCC 33591, the inoculation volume is 1 mL, and the test results are shown in Table 1 below.
  • the antibacterial properties of the spunlace nonwoven fabric prepared by the method of this application are good, especially for methicillin-resistant Staphylococcus aureus, which is more toxic and drug resistant, and its antibacterial properties are still relatively good.
  • the copper ion concentration in the initial organic complexed copper solution in this application is 5.5wt%, adding 10-30 volume multiples of water, combined with the control of the fiber material used for fiber web formation, can control the spunlace nonwoven
  • the amount of copper ions on the cloth is between 500ppm-8000ppm, which has a good antibacterial effect.
  • the spunlace non-woven fiber material in Examples 1-5 is a fiber containing hydroxyl groups.
  • the raw material of the spunlace non-woven fabric is synthetic polyester.
  • the fiber does not contain cellulose. It is first dipped in a chitosan-ascorbic acid solution and then dipped in an organic complex copper solution.
  • the final spunlace non-woven fabric also has good antibacterial properties.
  • Example 2 The spunlace non-woven fabrics obtained in Example 2, Example 7 and Comparative Examples 1 and 3 were washed 50 times, 100 times and 200 times, respectively, and then referenced to AATCC 100-2012 textile antibacterial performance test.
  • the test sample is the diameter It is a 4.8 cm disc, the tested strain is methicillin-resistant Staphylococcus aureus ATCC 33591, and the volume of the inoculation is 1 mL.
  • the copper content on the spunlace non-woven fabric is tested to determine the copper content loss, and the test The results are shown in Table 3 below.
  • the spunlace non-woven fabric prepared in Example 2 was tested for influenza A virus H1N1 according to the standard of ISO 18184:2014(E) "Anti-Virus Textile Testing".
  • the experimental group and the control group were set up, and the virus strain was prevented by China Influenza A virus A/PR8/34 (H1N1) provided by the Institute of Virology, Academy of Medical Sciences, the cell line is a continuous canine kidney epithelial cell line MDCK cells, purchased from ATCC, the logarithm value of the virus titer of the test group samples after inoculation and incubation for 24 hours (lgTCID 50 /bottle) The average value is 3.48, the antiviral activity value is 3.08, the antiviral activity rate is 99.92%, and the antiviral activity is good.
  • the copper-containing spunlace non-woven fabric prepared in this application was tested and evaluated for anti-virus, and mouse Noro s99 was used instead of human Norovirus to perform the inactivation residual activity test on human skin. It is verified that the copper-containing non-woven fabric can inactivate the virus on the human skin within 4 hours.
  • the experimental group and the control group are set up and 5 parallel tests are carried out.
  • the skin is provided by the human subcutaneous tissue of the British Tissue Solutions Limited company.
  • the virus is selected in Murine norovirus s99 Berlin strain/RAW cells stored at -80°C and isolated from mouse RAW cells, the virus number is MNV 260315.17, the test steps are as follows:
  • Example 2 Use the wet copper-containing spunlace nonwoven fabric prepared in Example 2 to perform standard wiping action on the surface of the subcutaneous tissue sample (1.0 ⁇ 1.0cm): fix the subcutaneous tissue sample with sterile tweezers, and then use the copper-containing spunlace The non-woven fabric wipes 3 times along the surface of the subcutaneous tissue sample, and wipes 3 times at 90°C, and then repeats this process for a duration of 30s.
  • the above-mentioned wiping process is carried out in a separate sterile plastic petri dish;
  • DMEM medium is Dulbecco's modified Eagle medium
  • a sample of the filtrate in a volume of 0.1ml was passed through gel filtration (Microspin S-400 HR chromatographic column), and the eluent was serially diluted 10 times for TCID 50 analysis.
  • TCID 50 was calculated for all 5 groups of parallel experiments.
  • TCID 50 is calculated according to the Karber method.
  • the virus in the eluate is calculated as 10 ( ⁇ n+0.5) ⁇ 400 TCID50/ml, where ⁇ n is the sum of the proportions of infected wells from 10 -1 to 10 -6 virus dilution.
  • the murine norovirus s99 Berlin strain/RAW cell was used as a substitute for human norovirus to perform a virus test on human skin.
  • the logarithmic value of the virus titer of the experimental group in Example 2 of this application (lgTCID 50 /bottle) The average value is 4.00, and the antiviral activity is good.
  • the biological activity of the virus on the human skin in the experimental group was reduced by 57.32% on average after the copper-containing spunlace non-woven fabric treatment, verifying that the human skin was wiped with the copper-containing spunlace non-woven fabric for 4 hours to inactivate the virus The effect verifies the excellent antiviral performance of the copper-containing spunlace non-woven fabric.
  • the spunlace non-woven fabric obtained by the method provided in this application has antibacterial and anti-viral properties, and can be widely used in medical and sanitary non-woven fabrics, non-woven fabrics for home decoration, non-woven fabrics for clothing, and non-woven fabrics for industrial use.
  • Fabrics, agricultural non-woven fabrics and other fields, especially using its antibacterial and antiviral properties in medical and health products such as masks, surgical gowns, etc. have a wide range of applications.

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Abstract

一种含铜抗菌、抗病毒无纺布及其制备方法，其制备方法包括以下步骤：将纤维料依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布；将水刺纤维布基布于有机络合铜溶液中浸轧上浆，得到含铜水刺无纺布，含铜水刺无纺布上铜含量≥500ppm；浸轧上浆后得到的含铜水刺无纺布进行烘干卷绕，该方法具有易实现工业化，流程简单，生产周期短的优点；通过上述方法制得的含铜抗菌、抗病毒无纺布，具有优异的抗菌抗病毒的性能；上述含铜抗菌、抗病毒无纺布的应用广泛。

Description

一种含铜抗菌、抗病毒无纺布及其制备方法 技术领域
本申请涉及无纺布的技术领域，更具体而言，其涉及一种含铜抗菌、抗病毒无纺布及其制备方法。
背景技术
随着大规模、高传染性的疾病快速传播，市场对抗菌非织造材料需求迅速提高，对非织造材料的抗菌性能也提出了更高的要求，开发具有良好抗菌、抑菌性能的非织造材料已成为当前非织布领域的热点之一。
水刺无纺布是将高压微细水流喷射到一层或多层纤维网上使纤维相互缠结而使纤网得以加固而具备一定强度的织物。因为其强度高、低起毛性、高吸湿性以及良好的透气性等优势，水刺无纺布已经成为近年来非织界技术进步最快的一个领域，被广泛应用于医疗、卫生用无纺布、家庭装饰用无纺布、服装用无纺布、工业用无纺布、农业用无纺布等领域。特别地，近年来，医疗卫生用无纺布需求量大大增加的同时，对其抑菌以及抗病毒的性能提出了更高的要求。
然而，无纺布因为其多孔式形状和高分子化合物的化学结构有利于微生物的附着，因此水刺无纺布的抗菌功能性研究和开发有着重要的意义。
发明内容
针对现有技术存在的不足，在第一方面，本申请提供了一种含铜抗菌、抗病毒无纺布的制备方法，其具有可以制备得到抗菌性好，还具有一定抗病毒的水刺无纺布且制备方法简单易实现工业化，流程简单的优点。
具体而言，本申请提供了如下技术方案：一种含铜抗菌、抗病毒无纺布的制备方法，包括以下步骤：
水刺无纺布基布制备：将纤维料依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布；
浸轧上浆：将水刺纤维布基布于有机络合铜溶液中浸轧上浆，得到含铜水刺无纺布，含铜水刺无纺布上铜含量≥500ppm；
浸轧上浆后得到的含铜水刺无纺布进行烘干卷绕。
通过采用上述技术方案，铜元素具有强效的杀菌功能，还具有一定的抗病毒效果，本申请将水刺无纺布于有机络合铜溶液中浸轧上浆，一方面使得有机 络合铜溶液不仅可以涂覆于水刺无纺布的表面，而且可以渗透进入水刺无纺布内部空隙内，使得水刺无纺布的内部尤其是纤维之间的空隙孔洞以及水刺无纺布的表面均有铜离子，从而可以起到更好的抗菌作用，另外一方面，铜元素以铜离子的形态存在于水刺无纺布的纤维之间，抗菌功能更为显著，尤其是含铜水刺无纺布上铜离子浓度的控制使得最终的水刺无纺布起到优良的抗菌抗病毒效果。
本申请中在水刺无纺布制备过程中，首先将纤维料纤维成网，然后预湿，然后进行水刺加固，纤网在水刺作用下，纤维间发生移动、穿插、缠结、抱合，形成无数个柔软的缠结点，使得纤网固结，得到水刺纤维布基布，预湿操作压实蓬松的纤网，排除纤网中的空气，使得纤网进入水刺区后能够有效吸收水射流的能量，加强纤维缠结效果，而且使得后续浸轧上浆时，有机络合铜溶液中铜离子可以更加牢固地镶嵌在纤维表面和纤维内部，加强铜离子与纤网之间的结合强度，最终得到的水刺无纺布的抗菌性能优异。
此外，相较于直接采用抗菌纤维制成的方式，本申请中水刺无纺布生产过程中其纤维成网以及水刺加固后直接进行浸轧上浆，一方面，操作更加简单方便，流程周期更短，可以在短时间内大规模生产水刺无纺布，满足供应，且可以满足无纺布的使用性能，而且抗菌抗病毒性能优良，将其应用于一次性医疗用品中，对于疫情期间针对各种医疗用品的需求供给具有重大的意义；另一方面在有机络合铜溶液中浸轧通过，使得水刺无纺布的各个间隙和区域之间浸润均匀，抗菌效果均一，可有效避免烘干后水刺无纺布孔洞内物质的沉淀。
本申请进一步设置为：所述纤维料包含天然纤维、人造纤维素纤维、人造蛋白质纤维、聚丙烯腈纤维、聚乙烯醇纤维中的至少一种。
通过采用上述技术方案，上述纤维料的分子结构中含有开放的羟基，形成的水刺纤维布基布中含有开放的羟基，将水刺纤维布基布于有机络合铜溶液中浸轧的时候，络合铜离子与纤维素或蛋白质纤维之间形成化学螯合，两者结合牢固，使用过程中不易脱落，水刺纤维布的抗菌持久性能优良。
本申请进一步设置为：纤维料纤维成网步骤后得到的布料含有≥5％的棉纤维，或5-65％的纤维素纤维，或5-65％的蛋白质纤维，或5-65％的聚丙烯腈纤维，或100％的低溶点聚乙烯醇纤维；
所述有机络合铜溶液由5.5wt％的初始有机络合铜溶液加入10-30体积倍数的水得到。
通过采用上述技术方案，通过对纤维成网步骤后得到的布料中棉纤维或纤维素纤维等纤维含量的控制以及有机络合铜溶液中铜离子浓度的控制，最终控制水刺纤维布上铜含量，起到优异的抗菌抗病毒性能。
此外，当布料为100％的低溶点聚乙烯醇纤维时，其可以在低温水中即可溶解，减小了废物产生，尤其是对于当前医疗废物垃圾处理起到了重要的意义。
本申请进一步设置为：初始有机络合铜溶液按照以下方法制得：
制备配位离子液体：将尿素、己内酰胺和乙酰胺均匀混合，然后加热保温直至己内酰胺和尿素均匀熔融液化，得到配位离子液体；
制备有机络合铜溶液：将包括氯化钠、高锰酸钾、过氧化钠和铜粉的配位固体混合物加入配位离子液体中搅拌均匀，反应，冷却后倒入纯水中得到铜含量为5.5wt％的初始有机络合铜溶液。
通过采用上述技术方案，本申请中将有机络合铜溶液用于水刺无纺布中，相较于无机铜，有机铜更加安全可靠，与环境相容性好，而且其相容性好，其抗菌功效持续时间长，且通过初始有机络合铜溶液中的铜离子浓度以及水的添加量可以控制最终水刺无纺布上的铜含量，最终起到优良的抗菌抗病毒性能。
本申请进一步设置为：配制配位离子液体步骤中，尿素、己内酰胺和乙酰胺的混合重量比为1：(0.2-0.4)：(0.2-0.4)，均匀混合后加热温度为100-120℃，保温时间为0.5-1h。
本申请进一步设置为：制备有机络合铜溶液步骤中：氯化钠、高锰酸钾、过氧化钠和铜粉的混合重量比为1：(1-2)：(1-2)：(2.5-2.9)，配位固体混合物和配位离子液体的混合重量比为1：(3-3.5)。
通过采用上述技术方案，制备有机络合铜溶液步骤中，通过控制氯酸钠、高锰酸钾、过氧化钠以及铜粉之间的质量比，使得铜粉全部氧化成一价离子，与配位离子液体中的有机物螯合形成络合铜。
本申请进一步设置为：当纤维料为聚酯纤维、聚酰胺纤维、聚氯乙烯纤维、聚丙烯纤维中的一种或几种的时候，水刺纤维布基布在浸轧上浆之前还进行壳聚糖-抗坏血酸溶液浸轧步骤，具体操作为：将水刺纤维布基布在壳聚糖-抗坏 血酸溶液中浸轧，然后在150-170℃下干燥5-10min，壳聚糖-抗坏血酸溶液的制备方法为：将5-10份壳聚糖粉加入25-30份醋酸和60-70份水中，磁力搅拌至壳聚糖溶解，然后再加入3-5份抗坏血酸，搅拌均匀。
通过采用上述技术方案，壳聚糖和抗坏血酸的分子结构均存在开放的羟基，将水刺纤维布基布首先在壳聚糖-抗坏血酸溶液中浸轧，壳聚糖和抗坏血酸浸入水刺纤维布的间隙中，增强水刺纤维布基布上的羟基结合点，后续在有机络合铜溶液中浸轧的时候与络合铜离子具有更多的结合位点。此外，相较于二价铜，一价铜配位键的共价性更强，故一价铜配合物的稳定性较二价铜配合物的稳定性更强，本申请中利用抗坏血酸的强还原性，加入抗坏血酸可以抑制一价铜被氧化为二价铜，从而增强抗菌性能以及抗菌等功能的持久性。
体系中还加入有壳聚糖，溶解后的壳聚糖具有较强的吸附能力，壳聚糖可以更加牢固地附在水刺纤维布基布之间，而且还可以提高抗坏血酸与水刺纤维布基布之间的结合强度。醋酸的加入一方面可以溶解壳聚糖，另一方面也可以增强壳聚糖与水刺纤维布基布之间的吸附，使得壳聚糖与抗坏血酸可以更加牢固地吸附在水刺纤维布基布上，然后再进行烘干操作后进行浸轧，此外，壳聚糖也有一定的抑菌性能以及优良的吸湿性能，可以进一步增强水刺纤维布的抗菌性能以及吸湿性能。
本申请进一步设置为：水刺纤维布基布在壳聚糖-抗坏血酸溶液浸轧步骤后还进行皂洗步骤，具体操作为：干燥后的水刺纤维布基布在5g/L的皂洗剂中皂洗5-10min，皂洗温度为35-40℃，然后在50-60℃下烘干。
通过采用上述技术方案，将壳聚糖-抗坏血酸溶液浸轧后的水刺纤维布基布进行皂洗，可以去掉水刺纤维布基布上结合不牢的壳聚糖和抗坏血酸，防止后续在浸轧的时候壳聚糖和抗坏血酸进入有机络合铜溶液中，与络合铜离子络合。
在第二方面，本申请提供了一种含铜抗菌、抗病毒无纺布，其具有抗菌性好，还具有一定抗病毒性能的优点。
具体而言，本申请提供了如下技术方案：一种含铜抗菌、抗病毒无纺布，由根据前述第一方面所述的制备方法制得。
通过采用上述技术方案，通过上述方法制得的水刺无纺布在保持水刺无纺 布具有优良的透气性和高吸湿性以及低起毛性的基础上改进了其抗菌性和抗病毒性能，得到的水刺无纺布的抗菌性、抗病毒性能优良，具有广泛的应用空间。
在第三方面，本申请提供了一种含铜抗菌、抗病毒无纺布的应用，其具有应用广泛的优点。
具体而言，本申请提供了如下技术方案：一种如上述的含铜抗菌、抗病毒无纺布在医疗卫生用品的应用。
通过采用上述技术方案，本申请中得到的无纺布具有优良的抗菌抗病性性能，在医疗卫生用品如手术服、手术罩布、医用包扎材料、伤口敷料、医用纱布以及口罩等产品具有广泛的应用。
综上所述，本申请具有以下有益效果：
1、本申请中利用铜元素的杀菌效果以及抗病毒效果，将水刺无纺布于有机络合铜溶液中浸轧上浆，一方面，铜元素以络合铜离子的形态存在于水刺无纺布的纤维之间，抗菌功能更为显著，尤其是通过控制水刺无纺布上的铜离子浓度，起到抗菌抗病毒的效果，此外，有机络合铜溶液不仅可以涂覆于水刺无纺布的表面，而且可以渗透进入水刺无纺布内部空隙内，使得水刺无纺布的内部尤其是纤维之间的空隙孔洞以及水刺无纺布的表面均有铜离子，从而可以起到更好的抗菌作用；
2、相较于直接采用抗菌纤维制成的方式，本申请中水刺无纺布生产过程中其纤维成网以及水刺加固后直接进行浸轧上浆，一方面，在有机络合铜溶液中浸轧通过，使得水刺无纺布的各个间隙和区域之间浸润均匀，抗菌效果均一，可有效避免烘干后水刺无纺布孔洞内物质的沉淀；另一方面，操作更加简单方便，流程周期更短，可以在短时间内大规模生产水刺无纺布，满足供应，且可以满足无纺布的使用性能，而且抗菌抗病毒性能优良，将其应用于一次性医疗用品中，对于疫情期间针对各种医疗用品的需求供给具有重大的意义；
3、本申请中用于纤维成网的纤维料包含天然纤维、人造纤维素纤维、人造蛋白质纤维、聚丙烯腈纤维、聚乙烯醇纤维中的至少一种，使得水刺纤维布基布中含有开放的羟基，后续在有机络合铜溶液中浸轧的时候，络合铜与羟基之间形成化学螯合，两者结合牢固，使用过程中不易脱落，最终得到的水刺纤维布的抗菌持久性能优良。
具体实施方式
以下结合实施例对本申请的实施方案进行详细描述，但是本领域人员将理解，下列实施例仅用于说明本申请，而不应视为限制本申请的范围，实施例中未注明具体条件者，按照常规条件或制造商建议的条件进行。
需要说明的是：水刺工艺可以加工各种纤维，如棉纤维，尼龙纤维，聚丙烯纤维，聚酯纤维或粘胶纤维等常见纤维，因此本申请中水刺无纺布基布制备步骤中得到的水刺无纺布的材料不受限制，其可以是纤维素纤维如粘胶纤维等，也可以是蛋白质纤维如花生蛋白质纤维等，也可以是聚酯纤维(涤纶)、聚酰胺纤维(锦纶/尼龙)、聚丙烯腈纤维(腈纶)、聚氯乙烯纤维(氯纶)、聚丙烯纤维(丙纶)或聚乙烯醇纤维(维伦)，通过控制有机络合铜溶液中铜含量控制水刺纤维布上的铜含量≥500ppm，更加优选为1000-8000ppm。
为使有机络合铜溶液中的络合铜离子与水刺纤维布的纤维之间形成化学螯合，使得铜离子不易脱落，水刺纤维布的抗菌和抗菌持久性更加优良，本申请中水刺纤维布基布步骤中，用于纤维成网的纤维料中包含天然纤维或湿法纺丝得到的纤维中的任意一种，具体的，包含天然纤维如棉纤维、人造纤维素纤维、人造蛋白质纤维、聚丙烯腈纤维、聚乙烯醇纤维中的至少一种。上述纤维中均含有羟基，则其在成网帘上成网之后得到的布料中含有开放的羟基，在有机络合铜溶液中浸轧的时候可以与络合铜离子形成化学螯合，两者结合的更为紧密，如纤维料为只有粘胶纤维或只有花生蛋白质纤维，或是粘胶纤维和花生蛋白质纤维的混合，均可。更加优选的，纤维料纤维成网步骤后得到的布料含有≥5wt％的棉纤维，或5-65wt％的纤维素纤维，或5-65wt％的蛋白质纤维，或5-65wt％的聚丙烯腈纤维，或100％的低温水溶性聚乙烯醇纤维，可以选用上述任意一种，但是不限于上述方案。当纤维料选用上述含羟基的纤维以及不含羟基的纤维的混合纤维料时，纤维成网之后的布料中含羟基纤维之和达到对应最低含量即可，如纤维料选用棉纤维、粘胶纤维和聚酯纤维的时候，只需要保证布料中棉纤维和粘胶纤维之和≥5wt％即可，比如纤维料选用粘胶纤维、聚丙烯腈纤维和聚酯纤维的时候，只需要保证布料中粘胶纤维和聚丙烯腈纤维之和为5-65wt％之间即可。通过对于布料中各个纤维含量的控制以及有机络合铜溶液中铜含量的控制，控制最终水刺纤维布上的铜含量。
上述低温水溶性聚乙烯醇纤维可以直接在低温水中溶解，可以在20-98℃的水中溶解。
当用于纤维成网的纤维料中没有羟基时，如纤维料中含有聚酯纤维、聚酰胺纤维、聚氯乙烯纤维、聚丙烯纤维中的一种或几种的时候，为了提高络合铜离子与水刺纤维布之间的结合强度，本申请中在浸轧上浆之前还进行壳聚糖-抗坏血酸溶液浸轧步骤，壳聚糖和抗坏血酸中均含有开放的羟基，再利用壳聚糖的吸附性能以及壳聚糖-抗坏血酸溶液中醋酸的加入将壳聚糖和抗坏血酸更加牢固的附着在水刺纤维布基布上，与有机络合铜溶液中络合铜离子形成化学螯合，增强有机铜与水刺纤维布之间的结合强度。
下面结合制备例、实施例和对比例对本申请做进一步详细的说明。
制备例1-5为有机络合铜溶液的制备例。
制备例1
一种有机络合铜溶液的制备方法，包括以下步骤：
S1、制备配位离子液体：将尿素、己内酰胺和乙酰胺按照重量比为1：0.2：0.2均匀混合，然后加热至100℃，在100℃下保温1h，直至己内酰胺和尿素均匀熔融液化，得到配位离子液体；
S2、制备有机络合铜溶液：按照1：1：1：2.5的质量比称取氯化钠、高锰酸钾、过氧化钠和铜粉，混合得到配位固体混合物，然后将配位固体混合物加入到配位离子液体中搅拌均匀，配位固体混合物和配位离子液体的混合重量比为1：3，反应使铜粉完全氧化成一价离子并与上述配位离子液体中的有机物形成配位离子，冷却后倒入纯水中，配制为含铜量为5.5％的初始有机络合铜溶液，放置3天后未出现沉淀或者变色，将初始有机络合铜溶液倒入10体积倍数的纯水中，配制得到有机络合铜溶液。
制备例2
一种有机络合铜溶液的制备方法，包括以下步骤：
S1、制备配位离子液体：将尿素、己内酰胺和乙酰胺按照重量比为1：0.3：0.4均匀混合，然后加热至110℃，在110℃下保温0.5h，直至己内酰胺和尿素均匀熔融液化，得到配位离子液体；
S2、制备有机络合铜溶液：按照1：2：1：2.9的质量比称取氯化钠、高 锰酸钾、过氧化钠和铜粉，混合得到配位固体混合物，然后将配位固体混合物加入到配位离子液体中搅拌均匀，配位固体混合物和配位离子液体的混合重量比为1：3.5，反应使铜粉完全氧化成一价离子并与上述配位离子液体中的有机物形成配位离子，冷却后倒入纯水中，配制为含铜量为5.5％的初始有机络合铜溶液，放置3天后未出现沉淀或者变色，将初始有机络合铜溶液倒入20体积倍数的纯水中，配制得到有机络合铜溶液。
制备例3
一种有机络合铜溶液的制备方法，包括以下步骤：
S1、制备配位离子液体：将尿素、己内酰胺和乙酰胺按照重量比为1：0.4：0.4均匀混合，然后加热至120℃，在120℃下保温1h，直至己内酰胺和尿素均匀熔融液化，得到配位离子液体；
S2、制备有机络合铜溶液：按照1：2：2：2.9的质量比称取氯化钠、高锰酸钾、过氧化钠和铜粉，混合得到配位固体混合物，然后将配位固体混合物加入到配位离子液体中搅拌均匀，配位固体混合物和配位离子液体的混合重量比为1：3.5，反应使铜粉完全氧化成一价离子并与上述配位离子液体中的有机物形成配位离子，冷却后倒入纯水中，配制为含铜量为5.5％的初始有机络合铜溶液，放置3天后未出现沉淀或者变色，将初始有机络合铜溶液倒入30体积倍数的纯水中，配制得到有机络合铜溶液。
制备例4
一种有机络合铜溶液的制备方法，按照制备例2中方法进行，不同之处在于将初始有机络合铜溶液倒入15体积倍数的纯水中，配制得到有机络合铜溶液。
制备例5
一种有机络合铜溶液的制备方法，按照制备例2中方法进行，不同之处在于将初始有机络合铜溶液倒入25体积倍数的纯水中，配制得到有机络合铜溶液。
制备例6-10为壳聚糖-抗坏血酸溶液的制备例。
制备例6
一种壳聚糖-抗坏血酸溶液的制备方法，包括以下步骤：
将5kg壳聚糖粉加入25kg醋酸和60kg水中，磁力搅拌至壳聚糖溶解，然后再加入3kg抗坏血酸，搅拌均匀。
制备例7
一种壳聚糖-抗坏血酸溶液的制备方法，包括以下步骤：
将8kg壳聚糖粉加入28kg醋酸和65kg水中，磁力搅拌至壳聚糖溶解，然后再加入4kg抗坏血酸，搅拌均匀。
制备例8
一种壳聚糖-抗坏血酸溶液的制备方法，包括以下步骤：
将10kg壳聚糖粉加入30kg醋酸和70kg水中，磁力搅拌至壳聚糖溶解，然后再加入5kg抗坏血酸，搅拌均匀。
实施例
实施例1
一种含铜抗菌、抗病毒无纺布的制备方法，包括以下步骤：
水刺无纺布基布制备：将粘胶纤维和聚酯纤维混合纤维料依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布，纤维成网后的布料中含有5wt％的粘胶纤维；
浸轧上浆：通过上浆机将水刺纤维布基布于有机络合铜溶液中浸轧上浆，得到含铜水刺无纺布，上浆机中的有机络合铜溶液选用制备例2中制备得到的有机络合铜溶液；
浸轧上浆后得到的含铜水刺无纺布进行烘干卷绕，烘干温度为90℃。
实施例2
一种含铜抗菌、抗病毒无纺布的制备方法，包括以下步骤：
水刺无纺布基布制备：将粘胶纤维和聚丙烯腈纤维以及聚酯纤维混合纤维依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布，纤维成网后的布料中粘胶纤维和聚酯纤维之和为65wt％；
浸轧上浆：通过上浆机将水刺纤维布基布于有机络合铜溶液中浸轧上浆，得到含铜水刺无纺布，上浆机中的有机络合铜溶液选用制备例1中制备得到的有机络合铜溶液；
浸轧上浆后得到的含铜水刺无纺布进行烘干卷绕，烘干温度为100℃。
实施例3
一种含铜抗菌、抗病毒无纺布的制备方法，包括以下步骤：
水刺无纺布基布制备：将棉纤维和聚酯纤维混合纤维依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布，纤维成网后的布料中棉纤维含量为5wt％；
浸轧上浆：通过上浆机将水刺纤维布基布于有机络合铜溶液中浸轧上浆，得到含铜水刺无纺布，上浆机中的有机络合铜溶液选用制备例5中制备得到的有机络合铜溶液；
浸轧上浆后得到的含铜水刺无纺布进行烘干卷绕，烘干温度为100℃。
实施例4
一种含铜抗菌、抗病毒无纺布的制备方法，按照实施例2中的方法进行，不同之处在于，
水刺无纺布基布制备：将大豆纤维和聚酯纤维混合纤维依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布，纤维成网后的布料中大豆纤维含量为20wt％；
上浆机中的有机络合铜溶液选用制备例3中制备得到的有机络合铜溶液。
实施例5
一种含铜抗菌、抗病毒无纺布的制备方法，按照实施例2中的方法进行，不同之处在于，
水刺无纺布基布制备：将低温水溶性聚乙烯醇纤维依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布，其中，低温水溶性聚乙烯醇能够在20℃的水温中溶解；
上浆机中的有机络合铜溶液选用制备例4中制备得到的有机络合铜溶液。
实施例6
一种含铜抗菌、抗病毒无纺布的制备方法，包括以下步骤：
水刺无纺布基布制备：将聚丙烯纤维依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布；
壳聚糖-抗坏血酸溶液浸轧：于上浆机中将水刺纤维布基布在壳聚糖-抗坏血酸溶液中浸轧，然后在150℃下干燥10min，上浆机中的壳聚糖-抗坏血酸溶液选用制备例6制备得到的壳聚糖-抗坏血酸溶液；
皂洗：干燥后的水刺纤维布基布在5g/L的皂洗剂中皂洗10min，皂洗温度为35℃，然后在50℃下烘干，其中，皂洗剂购自东莞纺链新材料科技有限公司，品牌为纺链Texchain，型号为605；
浸轧上浆：通过上浆机将皂洗后的水刺纤维布基布于有机络合铜溶液中浸轧上浆，得到含铜水刺无纺布，上浆机中的有机络合铜溶液选用制备例1中制备得到的有机络合铜溶液；
浸轧上浆后得到的含铜水刺无纺布进行烘干卷绕，烘干温度为100℃。
实施例7
一种含铜抗菌、抗病毒无纺布的制备方法，包括以下步骤：
水刺无纺布基布制备：将聚酰胺纤维依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布；
壳聚糖-抗坏血酸溶液浸轧：于上浆机中将水刺纤维布基布在壳聚糖-抗坏血酸溶液中浸轧，然后在160℃下干燥8min，上浆机中的壳聚糖-抗坏血酸溶液选用制备例7制备得到的壳聚糖-抗坏血酸溶液；
皂洗：干燥后的水刺纤维布基布在5g/L的皂洗剂中皂洗5min，皂洗温度为40℃，然后在55℃下烘干，其中，皂洗剂购自东莞纺链新材料科技有限公司，品牌为纺链Texchain，型号为605；
浸轧上浆：通过上浆机将皂洗后的水刺纤维布基布于有机络合铜溶液中浸轧上浆，得到含铜水刺无纺布，上浆机中的有机络合铜溶液选用制备例2中制备得到的有机络合铜溶液；
浸轧上浆后得到的含铜水刺无纺布进行烘干卷绕，烘干温度为100℃。
实施例8
一种含铜抗菌、抗病毒无纺布的制备方法，包括以下步骤：
水刺无纺布基布制备：将聚氯乙烯纤维依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布；
壳聚糖-抗坏血酸溶液浸轧：于上浆机中将水刺纤维布基布在壳聚糖-抗坏血酸溶液中浸轧，然后在170℃下干燥5min，上浆机中的壳聚糖-抗坏血酸溶液选用制备例8制备得到的壳聚糖-抗坏血酸溶液；
皂洗：干燥后的水刺纤维布基布在5g/L的皂洗剂中皂洗5min，皂洗温度 为40℃，然后在60℃下烘干，其中，皂洗剂购自东莞纺链新材料科技有限公司，品牌为纺链Texchain，型号为605；
浸轧上浆：通过上浆机将皂洗后的水刺纤维布基布于有机络合铜溶液中浸轧上浆，得到含铜水刺无纺布，上浆机中的有机络合铜溶液选用制备例3中制备得到的有机络合铜溶液；
浸轧上浆后得到的含铜水刺无纺布进行烘干卷绕，烘干温度为100℃。
对比例
对比例1
一种含铜抗菌、抗病毒无纺布的制备方法，按照实施例2中方法进行，不同之处在于，浸轧上浆步骤中，上浆机中的有机络合铜溶液制备的时候，将初始有机络合铜溶液倒入12体积倍数的纯水中，其余与制备例2中相同。
对比例2
一种含铜抗菌、抗病毒无纺布的制备方法，按照实施例2中方法进行，不同之处在于，浸轧上浆步骤中，上浆机中的有机络合铜溶液制备的时候，将初始有机络合铜溶液倒入25体积倍数的纯水中，其余与制备例2中相同。
对比例3
一种含铜抗菌、抗病毒无纺布的制备方法，按照实施例2中方法进行，不同之处在于，浸轧上浆步骤中，上浆机中的溶液不是有机络合铜溶液，而是3mol/L的氯化铜溶液。
性能检测
1、抗菌试验检测
按照AATCC 100-2012纺织品抗菌性能检测实施例1-8中得到的水刺纤维布的抗菌性能，测试样品为直径是4.8cm的圆片，做4次平行试验，取平均值，检测菌种为耐甲氧西林金黄色葡萄球菌ATCC 33591，接种菌液体积为1mL，检测结果如下下表1所示。
表1实施例抗菌性能
Figure PCTCN2021077409-appb-000001
Figure PCTCN2021077409-appb-000002
同理，对对比例1-3中得到的水刺纤维布进行上述抗菌性能检测，检测如下表2所示。
表2对比例抗菌性能
Figure PCTCN2021077409-appb-000003
由上表1可知，通过采用本申请的方法制得的水刺无纺布的抗菌性能良好，尤其是针对毒性较强、耐药性的耐甲氧西林金黄色葡萄球菌，其抗菌性能依然较强，本申请中的初始有机络合铜溶液中的铜离子浓度为5.5wt％，添加10-30体积倍数的水，结合对用于纤维成网的纤维料的控制，可以控制水刺无纺布上的铜离子数量处于500ppm-8000ppm之间，起到良好的抗菌效果。再结合对比例3以及实施例2，可以看出采用本申请中的有机络合铜离子相较于直接添加无机铜，其抗菌性能大大提升，再参考对比例1-2以及实施例2的设置，可以 看出当有机络合铜溶液中铜离子浓度太低的时候，其抗菌效果大打折扣，铜离子浓度太高的时候，一方面抗菌性能不变，但是成本提高，且铜含量过高对于人体不利。
此外，实施例1-5中水刺无纺布纤维料为含有羟基的纤维，其直接在有机络合铜溶液中浸轧的时候，其抗菌效能高，而水刺无纺布原料涤纶为合成纤维，不含纤维素，其采用先在壳聚糖-抗坏血酸溶液中浸轧，再在有机络合铜溶液中浸轧，最终得到的水刺无纺布也具有良好的抗菌性能。
2、持久性能
将实施例2、实施例7以及对比例1、3中得到的水刺无纺布分别洗涤50次、100次和200次后再参照AATCC 100-2012纺织品抗菌性能检测抗菌性能，测试样品为直径是4.8cm的圆片，检测菌种为耐甲氧西林金黄色葡萄球菌ATCC 33591，接种菌液体积为1mL，此外，对于水刺无纺布上的铜含量进行检测，测定铜含量损失，检测结果如下表3所示。
表3耐久性能检测
Figure PCTCN2021077409-appb-000004
由上表3可以看出，在经过50次、100次和200次洗涤后，本申请得到的水刺无纺布对于耐甲氧西林金黄色葡萄球菌的抗菌作用并没有产生明显变化，本申请提供的方法得到的水刺无纺布的抗菌耐久性优良。
3、抗病毒检测
3.1、甲型流感病毒H1N1病毒检测
对实施例2中制得的水刺无纺布按照ISO 18184：2014(E)《抗病毒纺织品测试》标准进行甲型流感病毒H1N1病毒检测，设置实验组和对照组，病毒 株为由中国预防医学科学院病毒研究所提供的甲型流感病毒A/PR8/34(H1N1)，细胞株为犬肾上皮连续细胞系MDCK细胞，购自ATCC，试验组试样接种孵育24h后病毒滴度的对数值(lgTCID 50/瓶)平均值为3.48，抗病毒活性值为3.08，抗病毒活性率为99.92％，抗病毒活性效果好。
3.2、诺如病毒检测
通过英国Blu Test Laboratories实验室对本申请制得的含铜水刺无纺布进行抗病毒测试和评定，选用小鼠诺如s99代替人体诺如病毒在人体皮肤上进行灭活残留的活性试验，以验证含铜无纺布可在4h内使人体皮肤上的病毒失活，设置实验组和对照组并进行5组平行试验，其中，皮肤由英国Tissue Solutions Limited公司提供的人体皮下组织，病毒选用在-80℃下保存、从小鼠RAW细胞中分离的鼠诺如病毒s99 Berlin株/RAW细胞，病毒编号为MNV 260315.17，试验步骤如下：
使用实施例2中制备得到的湿含铜水刺无纺布在皮下组织试样(1.0×1.0cm)表面进行标准擦拭动作：用无菌镊子将皮下组织试样固定，然后用含铜水刺无纺布沿着皮下组织试样表面擦拭3下为一遍，在90℃下擦拭三遍，然后重复此过程，持续时间为30s，上述擦拭过程在单独的无菌塑料培养皿中进行；
在室温下培育4小时后，将50μl病毒悬浮液接种到皮下组织试样表面1分钟；
将皮下组织试样转移至2.0ml冷细胞培养基(DMEM培养基+5.0％V/V胎牛血清，其中DMEM培养基为Dulbecco改良Eagle培养基)中并加入1.0g无菌玻璃珠，涡旋20秒；然后通过0.45um过滤器过滤分离，分离后滤液在-20℃下储存过夜。取0.1ml体积滤液样品通过凝胶过滤(Microspin S-400 HR色谱柱)，并将洗脱液连续稀释10倍以进行TCID 50分析。
对5组平行试验均进行TCID 50计算。
TCID 50根据Karber法计算。
洗脱液中病毒按10 (∑n+0.5)×400 TCID50/ml计算，其中∑n是从10 -1到10 -6病毒稀释度感染的孔的比例之和。
经过检测，鼠诺如病毒s99 Berlin株/RAW细胞作为人类诺如病毒的替代品在人体皮肤上进行病毒试验，本申请中实施例2实验组的病毒滴度的对数值 (lgTCID 50/瓶)平均值为4.00，抗病毒活性效果好。且与对照组相比较，实验组经过含铜水刺无纺布处理后人体皮肤上病毒的生物活性平均降低57.32％，验证人体皮肤在含铜水刺无纺布擦拭4h后对于病毒的灭活效果，验证了含铜水刺无纺布优良的抗病毒性能。
综上，本申请提供的方法获得的水刺无纺布具有抗菌抗病毒性能，可以广泛应用于医疗、卫生用无纺布、家庭装饰用无纺布、服装用无纺布、工业用无纺布、农业用无纺布等领域，尤其利用其抗菌抗病毒性能在医疗卫生用品如口罩、手术服等具有广泛的应用。
本具体实施例仅仅是对本申请的解释，其并不是对本申请的限制，本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改，但只要在本申请的权利要求范围内都受到专利法的保护。

Claims (9)

  1. 一种含铜抗菌、抗病毒无纺布的制备方法，其特征在于，包括以下步骤：
    水刺无纺布基布制备：将纤维料依次经过纤维成网、预湿、水刺加固后得到水刺纤维布基布；
    浸轧上浆：将水刺纤维布基布于有机络合铜溶液中浸轧上浆，得到含铜水刺无纺布，含铜水刺无纺布上铜含量≥500ppm；
    浸轧上浆后得到的含铜水刺无纺布进行烘干卷绕。
  2. 根据权利要求1所述的一种含铜抗菌、抗病毒无纺布的制备方法，其特征在于，所述纤维料包含天然纤维、人造纤维素纤维、人造蛋白质纤维、聚丙烯腈纤维、聚乙烯醇纤维中的至少一种。
  3. 根据权利要求1所述的一种含铜抗菌、抗病毒无纺布的制备方法，其特征在于，纤维料纤维成网步骤后得到的布料含有≥5％的棉纤维，或5-65％的纤维素纤维，或5-65％的蛋白质纤维，或5-65％的聚丙烯腈纤维，或100％的低温水溶性聚乙烯醇纤维；
    所述有机络合铜溶液由5.5wt％的初始有机络合铜溶液加入10-30体积倍数的水得到。
  4. 根据权利要求3所述的一种含铜抗菌、抗病毒无纺布的制备方法，其特征在于，初始有机络合铜溶液按照以下方法制得：
    制备配位离子液体：将尿素、己内酰胺和乙酰胺均匀混合，然后加热保温直至己内酰胺和尿素均匀熔融液化，得到配位离子液体；
    制备有机络合铜溶液：将包括氯化钠、高锰酸钾、过氧化钠和铜粉的配位固体混合物加入配位离子液体中搅拌均匀，反应，冷却后倒入纯水中得到铜含量为5.5wt％的初始有机络合铜溶液。
  5. 根据权利要求4所述的一种含铜抗菌、抗病毒无纺布的制备方法，其特征在于，配制配位离子液体步骤中，尿素、己内酰胺和乙酰胺的混合重量比为1：(0.2-0.4)：(0.2-0.4)，均匀混合后加热温度为100-120℃，保温时间为0.5-1h。
  6. 根据权利要求4所述的一种含铜抗菌、抗病毒无纺布的制备方法，其特征在于，制备有机络合铜溶液步骤中：氯化钠、高锰酸钾、过氧化钠和铜粉的混合重量比为1：(1-2)：(1-2)：(2.5-2.9)，配位固体混合物和配位离子液体的混合重量比为1：(3-3.5)。
  7. 根据权利要求1所述的一种含铜抗菌、抗病毒无纺布的制备方法，其特征在于，当纤维料为聚酯纤维、聚酰胺纤维、聚氯乙烯纤维、聚丙烯纤维中的一种或几种的时候，水刺纤维布基布在浸轧上浆之前还进行壳聚糖-抗坏血酸溶液浸轧步骤，具体操作为：将水刺纤维布基布在壳聚糖-抗坏血酸溶液中浸轧，然后在150-170℃下干燥5-10min，壳聚糖-抗坏血酸溶液的制备方法为：将5-10份壳聚糖粉加入25-30份醋酸和60-70份水中，磁力搅拌至壳聚糖溶解，然后再加入3-5份抗坏血酸，搅拌均匀。
  8. 根据权利要求7所述的一种含铜抗菌、抗病毒无纺布的制备方法，其特征在于，水刺纤维布基布在壳聚糖-抗坏血酸溶液浸轧步骤后还进行皂洗步骤，具体操作为：干燥后的水刺纤维布基布在5g/L的皂洗剂中皂洗5-10min，皂洗温度为35-40℃，然后在50-60℃下烘干。
  9. 一种含铜抗菌、抗病毒无纺布，其特征在于，由权利要求1所述的制备方法制得。
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