CN113684607A

CN113684607A - Copper-containing antibacterial and antiviral non-woven fabric and preparation method thereof

Info

Publication number: CN113684607A
Application number: CN202010427848.8A
Authority: CN
Inventors: 许东东
Original assignee: Harvest Spf Textile Co ltd
Current assignee: Harvest Spf Textile Co ltd
Priority date: 2020-05-19
Filing date: 2020-05-19
Publication date: 2021-11-23
Also published as: WO2021232870A1; US20210363689A1

Abstract

The invention discloses a copper-containing antibacterial and antiviral non-woven fabric and a preparation method thereof, wherein the preparation method comprises the following steps: sequentially performing fiber web formation, prewetting and spunlace reinforcement on the fiber material to obtain spunlace fiber cloth base cloth; padding and sizing the spunlace fiber cloth base cloth in an organic complexing copper solution to obtain copper-containing spunlace non-woven fabric, wherein the copper content of the copper-containing spunlace non-woven fabric is more than or equal to 500 ppm; the copper-containing spunlace non-woven fabric obtained after padding and sizing is dried and wound, and the method has the advantages of simplicity, easy industrialization realization, simple flow and short production period; the invention also discloses the copper-containing antibacterial and antiviral non-woven fabric prepared by the method, which has excellent antibacterial and antiviral properties; the invention also discloses application of the copper-containing antibacterial and antiviral non-woven fabric, and has the advantage of wide application.

Description

Copper-containing antibacterial and antiviral non-woven fabric and preparation method thereof

Technical Field

The invention relates to the technical field of non-woven fabrics, in particular to a copper-containing antibacterial and anti-virus non-woven fabric and a preparation method thereof.

Background

The market demand for antibacterial non-woven materials is rapidly increased, higher requirements are put forward for the antibacterial performance of the non-woven materials, and the development of the non-woven materials with good antibacterial and bacteriostatic performance becomes one of the hot spots in the field of the current non-woven fabrics.

A spunlace nonwoven fabric is a fabric having a certain strength by jetting high-pressure fine water streams onto one or more fiber webs to entangle the fibers with each other, thereby reinforcing the fiber webs. Because of their advantages such as high strength, low fuzz, high moisture absorption, and good air permeability, spunlace nonwoven fabrics have become the fastest technical field in the nonwoven industry in recent years, and have been widely used in the fields of medical and sanitary nonwoven fabrics, home decoration nonwoven fabrics, clothing nonwoven fabrics, industrial nonwoven fabrics, agricultural nonwoven fabrics, and the like. The demand of the non-woven fabrics for medical and health is greatly increased, and simultaneously, higher requirements on the bacteriostatic and antiviral properties of the non-woven fabrics are provided. However, since the nonwoven fabric has a porous shape and a chemical structure of a polymer compound, which is advantageous for the attachment of microorganisms, research and development of antibacterial functionality of the spunlace nonwoven fabric are of great significance.

Disclosure of Invention

Aiming at the defects in the prior art, in the first aspect, the invention provides a preparation method of copper-containing antibacterial and antiviral non-woven fabric, which has the advantages that the antibacterial property is good, the water-jet non-woven fabric with certain antivirus is obtained, the preparation method is simple, the industrialization is easy to realize, and the process is simple.

Specifically, the invention provides the following technical scheme: a preparation method of copper-containing antibacterial and antiviral non-woven fabric comprises the following steps:

preparing a spunlace non-woven fabric base fabric: sequentially performing fiber web formation, prewetting and spunlace reinforcement on the fiber material to obtain spunlace fiber cloth base cloth;

padding and sizing: padding and sizing the spunlace fiber cloth base cloth in an organic complexing copper solution to obtain copper-containing spunlace non-woven cloth, wherein the copper content of the copper-containing spunlace non-woven cloth is more than or equal to 500 ppm;

and (4) drying and winding the copper-containing spunlace non-woven fabric obtained after padding and sizing.

By adopting the technical scheme, the copper element has a powerful sterilization function and also has a certain anti-virus effect, the spunlace nonwoven fabric is padded and sized in the organic complexing copper solution, on one hand, the organic complexing copper solution can be coated on the surface of the spunlace nonwoven fabric and can permeate into the internal gaps of the spunlace nonwoven fabric, and copper ions are arranged in the spunlace nonwoven fabric, especially in the gaps and holes between fibers and on the surface of the spunlace nonwoven fabric, so that a better antibacterial effect can be achieved.

In the preparation process of the spunlace non-woven fabric, fiber material fibers are firstly formed into a net, then prewetted and then spunlaced and reinforced, the fiber net moves, penetrates, entangles and coheres among the fibers under the action of spunlace to form a plurality of soft entanglement points, so that the fiber net is consolidated to obtain a spunlace fiber cloth base fabric, the prewetting operation is carried out to compact the fluffy fiber net and remove air in the fiber net, the fiber net can effectively absorb the energy of water jet after entering a spunlace area, the fiber entanglement effect is enhanced, and copper ions in an organic complexing copper solution can be more firmly embedded on the surfaces of the fibers and the interiors of the fibers during subsequent padding and sizing, the bonding strength between the copper ions and the fiber net is enhanced, and the finally obtained spunlace non-woven fabric has excellent antibacterial performance.

In addition, compared with a mode of directly adopting antibacterial fibers, the method has the advantages that the fiber is formed into a net in the production process of the spunlace non-woven fabric, and the spunlace non-woven fabric is directly subjected to padding and sizing after being subjected to spunlace reinforcement, on one hand, the operation is simpler and more convenient, the flow cycle is shorter, the spunlace non-woven fabric can be produced in a large scale in a short time, the supply is met, the service performance of the non-woven fabric can be met, the antibacterial and antiviral performances are excellent, the method is applied to disposable medical supplies, and the method has great significance for the demand supply of various medical supplies in an epidemic situation period; on the other hand, the spunlace nonwoven fabric is soaked and passed through in the organic complex copper solution, so that the gaps and the areas of the spunlace nonwoven fabric are soaked uniformly, the antibacterial effect is uniform, and the precipitation of substances in the holes of the spunlace nonwoven fabric after drying can be effectively avoided.

The invention is further configured to: the fiber material comprises at least one of natural fiber, man-made cellulose fiber, man-made protein fiber, polyacrylonitrile fiber and polyvinyl alcohol fiber.

By adopting the technical scheme, the molecular structure of the fiber material contains open hydroxyl, the formed spunlace fiber cloth base cloth contains open hydroxyl, and when the spunlace fiber cloth base cloth is padded in an organic complexing copper solution, chemical chelation is formed between complexing copper ions and cellulose or protein fibers, so that the two are firmly combined, the fibers are not easy to fall off in the using process, and the antibacterial lasting performance of the spunlace fiber cloth is excellent.

The invention is further configured to: the cloth obtained after the fiber material fiber web forming step contains more than or equal to 5 percent of cotton fiber, or 5 to 65 percent of cellulose fiber, or 5 to 65 percent of protein fiber, or 5 to 65 percent of polyacrylonitrile fiber, or 100 percent of low melting point polyvinyl alcohol fiber;

the organic complex copper solution is obtained by adding 5.5wt% of initial organic complex copper solution into 10-30 volume times of water.

By adopting the technical scheme, the copper content on the spunlace fiber cloth is finally controlled by controlling the content of fibers such as cotton fibers or cellulose fibers in the cloth obtained after the fiber-forming step and the concentration of copper ions in the organic complex copper solution, so that excellent antibacterial and antiviral properties are achieved.

In addition, when the cloth is 100% of the polyvinyl alcohol fiber with low melting point, the polyvinyl alcohol fiber can be dissolved in low-temperature water, so that the generation of wastes is reduced, and the cloth plays an important role in the current treatment of medical waste and garbage.

The invention is further configured to: the initial organic complex copper solution was prepared as follows:

preparing a coordination ionic liquid: uniformly mixing urea, caprolactam and acetamide, and then heating and preserving heat until the caprolactam and the urea are uniformly melted and liquefied to obtain coordination ionic liquid;

preparing an organic copper complex solution: adding a coordination solid mixture comprising sodium chloride, potassium permanganate, sodium peroxide and copper powder into the coordination ionic liquid, uniformly stirring, reacting, cooling, and pouring into pure water to obtain an initial organic complex copper solution with the copper content of 5.5 wt%.

By adopting the technical scheme, the organic complex copper solution is used in the spunlace non-woven fabric, compared with inorganic copper, the organic copper is safer and more reliable, has good compatibility with the environment and long duration of antibacterial effect, and the copper content of the final spunlace non-woven fabric can be controlled by the copper ion concentration in the initial organic complex copper solution and the addition of water, thereby finally achieving excellent antibacterial and antiviral properties.

The invention is further configured to: 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), the heating temperature is 100 ℃ and 120 ℃ after uniform mixing, and the heat preservation time is 0.5-1 h.

The invention is further configured to: the step of preparing the organic complex copper solution comprises the following steps: the mixing weight ratio of the sodium chloride, the potassium permanganate, the sodium peroxide and the copper powder is 1: (1-2): (1-2): (2.5-2.9), wherein the mixing weight ratio of the coordination solid mixture to the coordination ionic liquid is 1: (3-3.5).

By adopting the technical scheme, in the step of preparing the organic complex copper solution, the copper powder is completely oxidized into monovalent ions by controlling the mass ratio of the sodium chlorate, the potassium permanganate, the sodium peroxide and the copper powder, and the monovalent ions are chelated with organic matters in the coordination ionic liquid to form complex copper.

The invention is further configured to: when the fiber material is one or more of polyester fiber, polyamide fiber, polyvinyl chloride fiber and polypropylene fiber, the spunlace fiber cloth base cloth is further subjected to a chitosan-ascorbic acid solution padding step before padding and sizing, and the concrete operations are as follows: the preparation method comprises the following steps of padding spunlace fiber cloth base cloth in chitosan-ascorbic acid solution, and drying at the temperature of 150-: adding 5-10 parts of chitosan powder into 25-30 parts of acetic acid and 60-70 parts of water, magnetically stirring until the chitosan is dissolved, then adding 3-5 parts of ascorbic acid, and uniformly stirring.

By adopting the technical scheme, the molecular structures of chitosan and ascorbic acid have open hydroxyl groups, the spunlace fiber cloth base cloth is firstly padded in a chitosan-ascorbic acid solution, the chitosan and ascorbic acid are immersed in gaps of the spunlace fiber cloth, hydroxyl bonding points on the spunlace fiber cloth base cloth are enhanced, and more bonding points are formed with complex copper ions during padding in an organic complex copper solution. In addition, compared with bivalent copper, the covalent property of the coordination bond of the monovalent copper is stronger, so that the stability of the monovalent copper complex is stronger than that of the bivalent copper complex.

The chitosan is added into the system, the dissolved chitosan has stronger adsorption capacity, the chitosan can be more firmly attached between the spunlace fiber cloth base fabrics, and the bonding strength between the ascorbic acid and the spunlace fiber cloth base fabrics can be improved. The acetic acid is added to dissolve the chitosan, and the adsorption between the chitosan and the spunlace fiber cloth base cloth is enhanced, so that the chitosan and the ascorbic acid can be more firmly adsorbed on the spunlace fiber cloth base cloth, then the spunlace fiber cloth base cloth is subjected to padding after drying operation, and in addition, the chitosan also has certain antibacterial performance and excellent moisture absorption performance, and the antibacterial performance and the moisture absorption performance of the spunlace fiber cloth can be further enhanced.

The invention is further configured to: the spunlace fiber cloth base cloth is further subjected to a soaping step after the chitosan-ascorbic acid solution padding step, and the concrete operations are as follows: soaping the dried spunlace fiber cloth base cloth in 5g/L soaping agent for 5-10min at 35-40 ℃, and then drying at 50-60 ℃.

By adopting the technical scheme, the spunlace fiber cloth base cloth which is padded by the chitosan-ascorbic acid solution is soaped, so that the chitosan and ascorbic acid which are not firmly combined on the spunlace fiber cloth base cloth can be removed, and the chitosan and ascorbic acid are prevented from entering the organic complexing copper solution and complexing with complexing copper ions in the subsequent padding process.

In a second aspect, the invention provides a copper-containing antibacterial and antiviral non-woven fabric, which has the advantages of good antibacterial property and certain antiviral property.

Specifically, the invention provides the following technical scheme: a copper-containing antibacterial and antiviral nonwoven fabric produced by the production method according to the first aspect.

By adopting the technical scheme, the antibacterial property and the anti-virus property of the spunlace non-woven fabric prepared by the method are improved on the basis of keeping the excellent air permeability, high hygroscopicity and low fuzzing property of the spunlace non-woven fabric, and the obtained spunlace non-woven fabric has excellent antibacterial property and anti-virus property and wide application space.

In a third aspect, the invention provides an application of the copper-containing antibacterial and antiviral non-woven fabric, which has the advantage of wide application.

Specifically, the invention provides the following technical scheme: an application of the copper-containing antibacterial and antiviral non-woven fabric in medical and sanitary products.

By adopting the technical scheme, the non-woven fabric obtained in the invention has excellent antibacterial and disease-resistant performances, and can be widely applied to products of medical and health products such as surgical gowns, surgical cover cloth, medical dressing materials, wound dressings, medical gauze, masks and the like.

In conclusion, the invention has the following beneficial effects:

1. according to the invention, the spunlace nonwoven fabric is padded and sized in the organic complex copper solution by utilizing the bactericidal effect and the antiviral effect of the copper element, on one hand, the copper element exists between fibers of the spunlace nonwoven fabric in a complex copper ion form, the antibacterial function is more obvious, and especially, the antibacterial and antiviral effect is achieved by controlling the concentration of the copper ions on the spunlace nonwoven fabric;

2. compared with the mode of directly preparing the antibacterial fiber, the fiber is directly subjected to padding and sizing after being subjected to web forming and spunlace reinforcement in the production process of the spunlace non-woven fabric, on one hand, the spunlace non-woven fabric passes through padding in an organic complex copper solution, so that all gaps and areas of the spunlace non-woven fabric are uniformly infiltrated, the antibacterial effect is uniform, and the precipitation of substances in the dried holes of the spunlace non-woven fabric can be effectively avoided; on the other hand, the operation is simpler and more convenient, the flow cycle is shorter, the spunlace non-woven fabric can be produced in a large scale in a short time, the supply is met, the service performance of the non-woven fabric can be met, the antibacterial and antiviral properties are excellent, and the spunlace non-woven fabric has great significance for the demand supply of various medical supplies during epidemic situations when being applied to disposable medical supplies;

3. the fiber material for fiber web forming comprises at least one of natural fiber, man-made cellulose fiber, man-made protein fiber, polyacrylonitrile fiber and polyvinyl alcohol fiber, so that the spunlace fiber cloth base cloth contains open hydroxyl, chemical chelation is formed between the complexing copper and the hydroxyl during subsequent padding in organic complexing copper solution, the combination of the two is firm, the fiber material is not easy to fall off in the using process, and the finally obtained spunlace fiber cloth has excellent antibacterial and lasting performance.

Detailed Description

Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and those not specifically noted in the examples are carried out according to conventional conditions or conditions suggested by the manufacturer.

It should be noted that: the spunlace process can process various fibers, such as common fibers of cotton fibers, nylon fibers, polypropylene fibers, polyester fibers or viscose fibers, and the like, so that the materials of the spunlace nonwoven fabric obtained in the preparation step of the spunlace nonwoven fabric base fabric are not limited, the spunlace nonwoven fabric can be cellulose fibers such as viscose fibers and the like, can also be protein fibers such as peanut protein fibers and the like, and can also be polyester fibers (terylene), polyamide fibers (polyamide/nylon), polyacrylonitrile fibers (acrylon), polyvinyl chloride fibers (polyvinyl chloride fibers), polypropylene fibers (polypropylene fibers) or polyvinyl alcohol fibers (vinylon), and the copper content on the spunlace nonwoven fabric is controlled to be more than or equal to 500ppm, more preferably to be 1000 plus 8000ppm by controlling the copper content in the organic complex copper solution.

In order to form chemical chelation between the complexing copper ions in the organic complexing copper solution and fibers of the spunlace fiber cloth, so that the copper ions are not easy to fall off, and the antibacterial property and the antibacterial durability of the spunlace fiber cloth are more excellent, in the step of the spunlace fiber cloth base cloth, fiber materials for fiber web forming comprise any one of natural fibers or fibers obtained by wet spinning, specifically at least one of natural fibers, man-made cellulose fibers, man-made protein fibers, polyacrylonitrile fibers and polyvinyl alcohol fibers, wherein the fibers all contain hydroxyl groups, so that the cloth obtained after the web forming on a web forming curtain contains open hydroxyl groups, and can form chemical chelation with the complexing copper ions when the spunlace fiber is dipped in the organic complexing copper solution, and the combination of the two is more compact, such as only viscose fibers or only peanut protein fibers, or a mixture of viscose and peanut protein fibers, more preferably, the fabric obtained after the fiber-forming step of the fiber material contains more than or equal to 5wt% of cotton fibers, or 5-65 wt% of cellulose fibers, or 5-65 wt% of protein fibers, or 5-65 wt% of polyacrylonitrile fibers, or 100% of low-temperature water-soluble polyvinyl alcohol fibers, which can be selected from any one of the above solutions, but is not limited to the above solution, when the fiber material is a mixture of the above fibers containing hydroxyl and fibers containing no hydroxyl, the sum of the fibers containing hydroxyl in the fabric after fiber-forming can reach the corresponding minimum content, for example, when the fiber material is cotton fibers, viscose and polyester fibers, the sum of the cotton fibers and the viscose in the fabric is only required to be more than or equal to 5wt%, for example, the fiber material is viscose, When the polyacrylonitrile fiber and the polyester fiber are used, the sum of the viscose fiber and the polyacrylonitrile fiber in the cloth is only required to be 5-65 wt%. And controlling the content of each fiber in the cloth and the content of copper in the organic complex copper solution to control the copper content on the final spunlace fiber cloth.

The low-temperature water-soluble polyvinyl alcohol fiber can be directly dissolved in low-temperature water and can be dissolved in water with the temperature of 20-98 ℃.

When the fiber material used for the fiber web is not provided with hydroxyl, for example when the fiber material contains one or more of polyester fiber, polyamide fiber, polyvinyl chloride fiber and polypropylene fiber, in order to improve the bonding strength between the complex copper ions and the spunlace fiber cloth, the invention also carries out a chitosan-ascorbic acid solution padding step before padding and sizing, wherein both chitosan and ascorbic acid contain open hydroxyl, and then the chitosan and ascorbic acid are more firmly attached to the spunlace fiber cloth base cloth by utilizing the adsorption performance of chitosan and the addition of acetic acid in the chitosan-ascorbic acid solution to form chemical chelation with the complex copper ions in the organic complex copper solution, so as to enhance the bonding strength between organic copper and the spunlace fiber cloth.

The present invention will be described in further detail with reference to the following preparation examples, examples and comparative examples.

Preparation examples 1 to 5 are preparation examples of the organic complex copper solution.

Preparation example 1

A preparation method of an organic complex copper solution comprises the following steps:

s1, preparing a coordination ionic liquid: urea, caprolactam and acetamide are mixed according to the weight ratio of 1: 0.2: 0.2, uniformly mixing, heating to 100 ℃, and keeping the temperature at 100 ℃ for 1h until caprolactam and urea are uniformly melted and liquefied to obtain coordination ionic liquid;

s2, preparing an organic complex copper solution: according to the following steps of 1: 1: 1: 2.5, mixing to obtain a coordination solid mixture, adding the coordination solid mixture into the coordination ionic liquid, and uniformly stirring, wherein the mixing weight ratio of the coordination solid mixture to the coordination ionic liquid is 1: and 3, reacting to enable the copper powder to be completely oxidized into univalent ions and form coordination ions with organic matters in the coordination ionic liquid, cooling, pouring into pure water to prepare an initial organic complex copper solution with the copper content of 5.5%, standing for 3 days without precipitation or color change, pouring the initial organic complex copper solution into pure water with the volume multiple of 10, and preparing to obtain the organic complex copper solution.

Preparation example 2

s1, preparing a coordination ionic liquid: urea, caprolactam and acetamide are mixed according to the weight ratio of 1: 0.3: 0.4, uniformly mixing, heating to 110 ℃, and keeping the temperature at 110 ℃ for 0.5h until caprolactam and urea are uniformly melted and liquefied to obtain coordination ionic liquid;

s2, preparing an organic complex copper solution: according to the following steps of 1: 2: 1: 2.9, mixing to obtain a coordination solid mixture, adding the coordination solid mixture into the coordination ionic liquid, and uniformly stirring, wherein the mixing weight ratio of the coordination solid mixture to the coordination ionic liquid is 1: and 3.5, reacting to enable the copper powder to be completely oxidized into univalent ions and form coordination ions with organic matters in the coordination ionic liquid, cooling, pouring into pure water to prepare an initial organic complex copper solution with the copper content of 5.5%, standing for 3 days without precipitation or discoloration, pouring the initial organic complex copper solution into pure water with the volume multiple of 20, and preparing to obtain the organic complex copper solution.

Preparation example 3

s1, preparing a coordination ionic liquid: urea, caprolactam and acetamide are mixed according to the weight ratio of 1: 0.4: 0.4, uniformly mixing, heating to 120 ℃, and keeping the temperature at 120 ℃ for 1h until caprolactam and urea are uniformly melted and liquefied to obtain coordination ionic liquid;

s2, preparing an organic complex copper solution: according to the following steps of 1: 2: 2: 2.9, mixing to obtain a coordination solid mixture, adding the coordination solid mixture into the coordination ionic liquid, and uniformly stirring, wherein the mixing weight ratio of the coordination solid mixture to the coordination ionic liquid is 1: and 3.5, reacting to enable the copper powder to be completely oxidized into univalent ions and form coordination ions with organic matters in the coordination ionic liquid, cooling, pouring into pure water to prepare an initial organic complex copper solution with the copper content of 5.5%, standing for 3 days without precipitation or discoloration, and pouring the initial organic complex copper solution into pure water with the volume multiple of 30 to prepare the organic complex copper solution.

Preparation example 4

A preparation method of an organic complex copper solution is carried out according to the method in preparation example 2, and is characterized in that the initial organic complex copper solution is poured into pure water with the volume multiple of 15 to prepare the organic complex copper solution.

Preparation example 5

A preparation method of an organic complex copper solution is carried out according to the method in preparation example 2, and is characterized in that the initial organic complex copper solution is poured into pure water with the volume multiple of 25 to prepare the organic complex copper solution.

Preparation examples 6 to 10 are preparation examples of chitosan-ascorbic acid solutions.

Preparation example 6

A preparation method of a chitosan-ascorbic acid solution comprises the following steps:

adding 5kg chitosan powder into 25kg acetic acid and 60kg water, magnetically stirring until chitosan is dissolved, then adding 3kg ascorbic acid, and stirring uniformly.

Preparation example 7

adding 8kg of chitosan powder into 28kg of acetic acid and 65kg of water, magnetically stirring until the chitosan is dissolved, then adding 4kg of ascorbic acid, and uniformly stirring.

Preparation example 8

adding 10kg chitosan powder into 30kg acetic acid and 70kg water, magnetically stirring until the chitosan is dissolved, then adding 5kg ascorbic acid, and uniformly stirring.

Examples

Example 1

A preparation method of copper-containing antibacterial and antiviral non-woven fabric comprises the following steps:

preparing a spunlace non-woven fabric base fabric: sequentially performing fiber web formation, prewetting and spunlace reinforcement on viscose fiber and polyester fiber mixed fiber materials to obtain spunlace fiber cloth base cloth, wherein the fiber web-formed cloth contains 5wt% of viscose fiber;

padding and sizing: padding and sizing the spunlace fiber cloth base cloth in an organic complexing copper solution through a sizing machine to obtain a copper-containing spunlace non-woven cloth, wherein the organic complexing copper solution in the sizing machine is the organic complexing copper solution prepared in the preparation example 2;

and (3) drying and winding the copper-containing spunlace non-woven fabric obtained after padding and sizing, wherein the drying temperature is 90 ℃.

Example 2

preparing a spunlace non-woven fabric base fabric: sequentially performing fiber web formation, prewetting and spunlace reinforcement on viscose fibers, polyacrylonitrile fibers and polyester fiber mixed fibers to obtain spunlace fiber cloth base cloth, wherein the sum of the viscose fibers and the polyester fibers in the fiber web-formed cloth is 65 wt%;

padding and sizing: padding and sizing the spunlace fiber cloth base cloth in an organic complexing copper solution through a sizing machine to obtain a copper-containing spunlace non-woven cloth, wherein the organic complexing copper solution in the sizing machine is the organic complexing copper solution prepared in the preparation example 1;

and (3) drying and winding the copper-containing spunlace non-woven fabric obtained after padding and sizing, wherein the drying temperature is 100 ℃.

Example 3

preparing a spunlace non-woven fabric base fabric: sequentially performing fiber web formation, prewetting and spunlace reinforcement on cotton fiber and polyester fiber mixed fiber to obtain spunlace fiber cloth base cloth, wherein the cotton fiber content in the fiber web-formed cloth is 5 wt%; padding and sizing: padding and sizing the spunlace fiber cloth base cloth in an organic complexing copper solution through a sizing machine to obtain a copper-containing spunlace non-woven cloth, wherein the organic complexing copper solution in the sizing machine is the organic complexing copper solution prepared in the preparation example 5;

Example 4

A process for the preparation of a copper-containing antibacterial, antiviral nonwoven fabric, carried out as in example 2, except that,

preparing a spunlace non-woven fabric base fabric: the method comprises the following steps of sequentially performing fiber web formation, prewetting and spunlace reinforcement on mixed fibers of soybean fibers and polyester fibers to obtain spunlace fiber cloth base cloth, wherein the content of the soybean fibers in the cloth subjected to fiber web formation is 20 wt%; the organic copper complex solution in the sizing machine is the organic copper complex solution prepared in preparation example 3.

Example 5

preparing a spunlace non-woven fabric base fabric: sequentially performing fiber web formation, prewetting and spunlace reinforcement on low-temperature water-soluble polyvinyl alcohol fibers to obtain spunlace fiber cloth base cloth, wherein the low-temperature water-soluble polyvinyl alcohol can be dissolved in water at the temperature of 20 ℃;

the organic copper complex solution prepared in preparation example 4 was used as the organic copper complex solution in the sizing machine.

Example 6

preparing a spunlace non-woven fabric base fabric: sequentially performing fiber web formation, prewetting and spunlace reinforcement on polypropylene fibers to obtain spunlace fiber cloth base cloth;

padding with a chitosan-ascorbic acid solution: padding the spunlace fiber cloth base cloth in a chitosan-ascorbic acid solution in a sizing machine, and then drying for 10min at 150 ℃, wherein the chitosan-ascorbic acid solution in the sizing machine is the chitosan-ascorbic acid solution prepared in the preparation example 6;

soaping: soaping the dried spunlace fiber cloth base cloth in a soaping agent of 5g/L for 10min at the soaping temperature of 35 ℃, and then drying at the temperature of 50 ℃, wherein the soaping agent is purchased from Dongguan new spinning material science and technology company, and is of a spinning Texchain brand with a model number of 605;

padding and sizing: padding and sizing the spunlace fiber cloth base cloth subjected to soaping in an organic complexing copper solution by using a sizing machine to obtain a copper-containing spunlace non-woven fabric, wherein the organic complexing copper solution in the sizing machine is the organic complexing copper solution prepared in preparation example 1;

Example 7

preparing a spunlace non-woven fabric base fabric: sequentially performing fiber web formation, prewetting and spunlace reinforcement on polyamide fibers to obtain spunlace fiber cloth base cloth;

padding with a chitosan-ascorbic acid solution: padding the spunlace fiber cloth base cloth in a chitosan-ascorbic acid solution in a sizing machine, and then drying for 8min at 160 ℃, wherein the chitosan-ascorbic acid solution in the sizing machine is the chitosan-ascorbic acid solution prepared in preparation example 7;

soaping: soaping the dried spunlace fiber cloth base cloth in a soaping agent of 5g/L for 5min at the soaping temperature of 40 ℃, and then drying at the temperature of 55 ℃, wherein the soaping agent is purchased from Dongguan new spinning material science and technology company, and is of a spinning Texchain brand with a model number of 605;

padding and sizing: padding and sizing the spunlace fiber cloth base cloth subjected to soaping in an organic complexing copper solution by using a sizing machine to obtain a copper-containing spunlace non-woven fabric, wherein the organic complexing copper solution in the sizing machine is the organic complexing copper solution prepared in preparation example 2;

Example 8

preparing a spunlace non-woven fabric base fabric: sequentially performing fiber web formation, prewetting and spunlace reinforcement on polyvinyl chloride fibers to obtain spunlace fiber cloth base cloth;

padding with a chitosan-ascorbic acid solution: padding the spunlace fiber cloth base cloth in a chitosan-ascorbic acid solution in a sizing machine, and then drying for 5min at 170 ℃, wherein the chitosan-ascorbic acid solution in the sizing machine is the chitosan-ascorbic acid solution prepared in preparation example 8;

soaping: soaping the dried spunlace fiber cloth base cloth in a soaping agent of 5g/L for 5min at the soaping temperature of 40 ℃, and then drying at the temperature of 60 ℃, wherein the soaping agent is purchased from Dongguan new spinning material science and technology company, and is of a spinning Texchain with the model number of 605;

padding and sizing: padding and sizing the spunlace fiber cloth base cloth subjected to soaping in an organic complexing copper solution by using a sizing machine to obtain a copper-containing spunlace non-woven fabric, wherein the organic complexing copper solution in the sizing machine is the organic complexing copper solution prepared in preparation example 3;

Comparative example 1

A preparation method of copper-containing antibacterial and antiviral non-woven fabric is carried out according to the method in the example 2, except that in the padding and sizing step, when preparing the organic complex copper solution in the sizing machine, the initial organic complex copper solution is poured into pure water with the volume being 12 times of the volume, and the rest is the same as that in the preparation example 2.

Comparative example 2

A preparation method of copper-containing antibacterial and antiviral non-woven fabric is carried out according to the method in the example 2, except that in the padding and sizing step, when preparing the organic complex copper solution in the sizing machine, the initial organic complex copper solution is poured into pure water with 25 volume times, and the rest is the same as the preparation example 2.

Comparative example 3

A preparation method of copper-containing antibacterial and antiviral non-woven fabric is carried out according to the method in the example 2, and the difference is that in the padding and sizing step, the solution in a sizing machine is not an organic complex copper solution, but a 3mol/L copper chloride solution.

Performance detection

1. Antibacterial test detection

The antibacterial performance of the spunlace fiber cloth obtained in examples 1-8 is detected according to the antibacterial performance of AATCC 100-.

TABLE 1 examples antimicrobial Properties

Similarly, the above antibacterial performance test was performed on the spunlace fiber cloth obtained in comparative examples 1 to 3, and the test is shown in table 2 below.

TABLE 2 comparative example antimicrobial Properties

As shown in the above table 1, the spunlace nonwoven fabric prepared by the method of the present invention has good antibacterial performance, especially still strong antibacterial performance against methicillin-resistant Staphylococcus aureus with strong toxicity and drug resistance, the concentration of copper ions in the initial organic complex copper solution in the present invention is 5.5wt%, 10-30 volume times of water is added, and the amount of copper ions on the spunlace nonwoven fabric can be controlled to be 500ppm-8000ppm by combining with the control of the fiber material for fiber web formation, so as to achieve good antibacterial effect. In combination with the comparative example 3 and the example 2, it can be seen that the antibacterial performance of the organic complex copper ions is greatly improved compared with that of the organic copper ions which are directly added, and with reference to the settings of the comparative examples 1-2 and the example 2, the antibacterial effect is greatly reduced when the concentration of the copper ions in the organic complex copper solution is too low, and when the concentration of the copper ions is too high, on one hand, the antibacterial performance is unchanged, but the cost is increased, and the copper content is too high, which is not beneficial to human bodies.

In addition, the fiber material of the spunlace nonwoven fabric in examples 1 to 5 is a fiber containing hydroxyl, and when the fiber material is directly padded in an organic complex copper solution, the antibacterial efficiency is high, while the raw material terylene of the spunlace nonwoven fabric is a synthetic fiber and does not contain cellulose, the spunlace nonwoven fabric is firstly padded in a chitosan-ascorbic acid solution and then padded in an organic complex copper solution, and finally the obtained spunlace nonwoven fabric also has good antibacterial performance.

2. Durability performance

The spunlace nonwoven fabrics obtained in the examples 2 and 7 and the comparative examples 1 and 3 are respectively washed for 50 times, 100 times and 200 times, and then the antibacterial performance is detected according to the antibacterial performance of the AATCC 100 + 2012 textile, the test sample is a round piece with the diameter of 4.8cm, the detection strain is methicillin-resistant staphylococcus aureus ATCC 33591, the volume of the inoculated bacterial liquid is 1mL, and in addition, the copper content on the spunlace nonwoven fabrics is detected, the copper content loss is measured, and the detection results are shown in the following table 3.

TABLE 3 durability test

As can be seen from table 3 above, after 50 times, 100 times and 200 times of washing, the antibacterial effect of the spunlace nonwoven fabric obtained by the method of the present invention on methicillin-resistant staphylococcus aureus does not change significantly, and the spunlace nonwoven fabric obtained by the method of the present invention has excellent antibacterial durability.

3. Antiviral assays

3.1 detection of influenza A H1N1 Virus

The hydroentangled nonwoven obtained in example 2 was treated according to ISO 18184: 2014(E) antiviral textile test Standard for detecting influenza A virus H1N1, setting an experimental group and a control group, wherein the virus strain is influenza A virus A/PR8/34(H1N1) provided by virus research of China academy of preventive medicine sciences, the cell strain is canine kidney epithelial continuous cell line MDCK cell purchased from ATCC, and the logarithmic value (lgTCID) of virus titer of test group samples inoculated and incubated for 24H is obtained₅₀Bottle) average value is 3.48, antiviral activity value is 3.08, antiviral activity rate is 99.92%, and antiviral activity effect is good.

3.2 detection of norovirus

The anti-virus Test and evaluation of the copper-containing spunlace nonwoven fabric prepared by the invention are carried out by British Blu Test Laboratories, mouse norovirus s99 is selected to replace the activity Test of the inactivation residue on human skin so as to verify that the copper-containing nonwoven fabric can inactivate the virus on the human skin within 4h, an experimental group and a control group are arranged and 5 groups of parallel tests are carried out, wherein the skin is human subcutaneous Tissue provided by the British tissues Limited, the virus is selected from mouse norovirus s99 Berlin strain/RAW cell which is preserved at-80 ℃ and separated from mouse RAW cell, the virus number is MNV 260315.17, and the Test steps are as follows: the wet copper-containing spunlace nonwoven prepared in example 2 was used to perform a standard wiping action on the surface of a subcutaneous tissue sample (1.0 × 1.0 cm): fixing the subcutaneous tissue sample with sterile forceps, wiping the subcutaneous tissue sample with copper-containing spunlace nonwoven fabric for 3 times along the surface of the subcutaneous tissue sample, wiping the subcutaneous tissue sample for three times at 90 ℃, and repeating the process for 30s, wherein the wiping process is performed in a separate sterile plastic culture dish;

after 4 hours incubation at room temperature, 50 μ l of the virus suspension was inoculated onto the surface of the subcutaneous tissue sample for 1 minute; subcutaneous tissue samples were transferred to 2.0ml of cold cell medium (DMEM medium + 5.0% V/V fetal bovine serum, wherein DMEM medium is Dulbecco's modified Eagle's medium) and 1.0g of sterile glass beads were added and vortexed for 20 seconds; the separation was then carried out by filtration through a 0.45um filter, and the filtrate after separation was stored overnight at-20 ℃. A0.1 ml volume sample of the filtrate was passed through gel filtration (Microspin S-400HR column) and the eluate was serially diluted 10-fold for TCID₅₀And (6) analyzing.

TCID was performed for all 5 parallel experiments₅₀And (4) calculating.

TCID₅₀Calculated according to the Karber method.

The virus content in the eluent is 10^(∑n+0.5)X 400TCID50/ml, where Σ n is from 10^-1To 10^-6The ratio of virus dilution infected wells.

Through detection, the murine norovirus s99 Berlin strain/RAW cells are used as a substitute for human norovirus to carry out virus tests on human skin, and the log value (lgTCID) of the virus titer of the experimental group of example 2 in the invention₅₀Bottle) average value is 4.00, and the antiviral activity effect is good. Compared with a control group, the biological activity of the virus on human skin treated by the copper-containing spunlace non-woven fabric is reduced by 57.32% on average, the inactivation effect of the human skin on the virus after the copper-containing spunlace non-woven fabric is wiped for 4 hours is verified, and the excellent antiviral performance of the copper-containing spunlace non-woven fabric is verified.

In conclusion, the spunlace nonwoven fabric obtained by the method provided by the invention has antibacterial and antiviral properties, can be widely applied to the fields of medical and sanitary nonwoven fabrics, household decorative nonwoven fabrics, clothing nonwoven fabrics, industrial nonwoven fabrics, agricultural nonwoven fabrics and the like, and particularly has wide application in medical and sanitary products such as masks, surgical gowns and the like by utilizing the antibacterial and antiviral properties of the spunlace nonwoven fabric.

The present embodiment is only illustrative and not restrictive, and those skilled in the art can make modifications to the embodiment without inventive contribution as required after reading the present specification, but all the modifications are protected by patent law within the scope of the appended claims.

Claims

1. A preparation method of copper-containing antibacterial and antiviral non-woven fabric is characterized by comprising the following steps:

padding and sizing: padding and sizing the spunlace fiber cloth base cloth in an organic complexing copper solution to obtain copper-containing spunlace non-woven fabric, wherein the copper content of the copper-containing spunlace non-woven fabric is more than or equal to 500 ppm;

2. The method of claim 1, wherein the fiber material comprises at least one of natural fiber, man-made cellulose fiber, man-made protein fiber, polyacrylonitrile fiber, and polyvinyl alcohol fiber.

3. The method for preparing the copper-containing antibacterial and antiviral non-woven fabric according to claim 1, wherein the cloth obtained after the fiber-forming step of the fiber material contains more than or equal to 5% of cotton fiber, or 5-65% of cellulose fiber, or 5-65% of protein fiber, or 5-65% of polyacrylonitrile fiber, or 100% of low-temperature water-soluble polyvinyl alcohol fiber;

4. The method for preparing the copper-containing antibacterial and antiviral non-woven fabric according to claim 3, wherein the initial organic complex copper solution is prepared by the following method:

5. The method for preparing the copper-containing antibacterial and antiviral non-woven fabric according to claim 4, wherein 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), the heating temperature is 100 ℃ and 120 ℃ after uniform mixing, and the heat preservation time is 0.5-1 h.

6. The method for preparing the copper-containing antibacterial and antiviral non-woven fabric according to claim 4, wherein the step of preparing the organic complex copper solution comprises the following steps: the mixing weight ratio of the sodium chloride, the potassium permanganate, the sodium peroxide and the copper powder is 1: (1-2): (1-2): (2.5-2.9), wherein the mixing weight ratio of the coordination solid mixture to the coordination ionic liquid is 1: (3-3.5).

7. The method for preparing the copper-containing antibacterial and antiviral non-woven fabric according to claim 1, wherein when the fiber material is one or more of polyester fiber, polyamide fiber, polyvinyl chloride fiber and polypropylene fiber, the spunlace fiber fabric base fabric is further subjected to a chitosan-ascorbic acid solution padding step before padding and sizing, and the method comprises the following specific operations: padding the spunlace fiber cloth base cloth in a chitosan-ascorbic acid solution, and then drying for 5-10min at the temperature of 150-: adding 5-10 parts of chitosan powder into 25-30 parts of acetic acid and 60-70 parts of water, magnetically stirring until the chitosan is dissolved, then adding 3-5 parts of ascorbic acid, and uniformly stirring.

8. The method for preparing the copper-containing antibacterial and antiviral non-woven fabric according to claim 7, wherein the step of soaping the spunlace fiber cloth base fabric after the step of padding with the chitosan-ascorbic acid solution is further performed, and the specific operations are as follows: soaping the dried spunlace fiber cloth base cloth in 5g/L soaping agent for 5-10min at 35-40 ℃, and then drying at 50-60 ℃.

9. A copper-containing antibacterial and antiviral nonwoven fabric, characterized by being produced by the production method according to any one of claims 1 to 8.