Patent Application
20210363689
This application claims the priority benefit of China application serial no. 202010427848.8, filed on May 19, 2020. The entirety of the above-mentioned patent application is hereby incorporated by reference herein and made a part of this specification.
This application relates to a field of a non-woven fabric, and more particularly, to a Cu-containing non-woven fabric and a method for preparing the same.
People have a rapidly increasing awareness on health and hygiene following the outbreak of the epidemic “COVID-19” in 2020. There is a sharply increasing demand for antibacterial non-woven materials on the market, and a higher requirement for the antibacterial property is also put forward, thus developing non-woven materials with a good antibacterial property has become one of the hot spots in the field of non-woven fabric.
A spunlace non-woven fabric is a fabric having a strength obtained by spraying tiny high-pressure water jets onto a fiber-web with one or more layers such that fibers entangle with each other to strengthen the fiber-web. Due to advantages such as high strength, low tendency to pill, high hygroscopicity, and good air permeability, the spunlace non-woven fabric has become one of the fastest-growing areas in non-woven technology in recent years, which is widely used in the fields of medical and health, domestic decoration, clothing, industry, agriculture or the like. Particularly, following the outbreak of the epidemic “COVID-19”, there is a sharply increasing demand for a non-woven fabric used in medical and health, and a higher requirement for antibacterial and antivirus properties is also put forward. A non-woven fabric facilitates the attachment of microorganisms thereon due to its porous characteristics and chemical structure of a polymer compound, thus the research and development of the antibacterial property of a spunlace non-woven fabric is of great importance.
At a first aspect, this application provides a method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties by which a spunlace non-woven fabric with a good antibacterial property as well as antivirus property is prepared. The method is simple to perform and easy for industrialization.
In one embodiment, a method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties is provided, including the following steps:
preparing a spunlace non-woven base fabric: forming a web from a fiber, pre-wetting the web, and spunlacing the web to obtain the spunlace non-woven base fabric;
padding and sizing: padding and sizing the spunlace non-woven base fabric in an organic copper complex solution to obtain a Cu-containing spunlace non-woven fabric, in which the Cu-containing spunlace non-woven fabric contains copper of ≥500 ppm; and
drying and winding the obtained Cu-containing spunlace non-woven fabric.
Copper element has a strong antibacterial effect as well as a certain antivirus effect. In this embodiment, the spunlace non-woven fabric is padded and sized in the organic copper complex solution. On one hand, the organic copper complex solution can not only be coated on the surface of the spunlace non-woven fabric, but also penetrate into pores inside the spunlace non-woven fabric, such that there are copper ions both on the surface and inside the spunlace non-woven fabric, especially in the voids between fibers, thereby providing a good antibacterial effect. On the other hand, the copper element are present in the form of copper ions between fibers of the spunlace non-woven fabric, thereby achieving an excellent antibacterial effect. Furthermore, the spunlace non-woven fabric may achieve excellent antibacterial and antiviral effects by controlling the concentration of the copper ion on the Cu-containing spunlace non-woven fabric.
During the process of preparing the spunlace non-woven fabric, a web is formed from a fiber, pre-wetted, and spunlaced. Under the action of the spunlacing, fibers move, interweave, entangle and cohere with each other, forming numerous soft entangling points to consolidate the web, after which the spunlace non-woven base fabric is obtained. The loose fiber-web is compacted and the air is removed from the web by the pre-wetting operation, such that the web can effectively absorb the energy of the water jets after entering the spunlace area, which improves the entangling effect between fibers. Moreover, during the process of subsequent padding and sizing, copper ions in the organic composition copper solution can be more firmly attached on the surface and inside the fiber, which enhances the bonding between copper ions and the fiber-web, thus prepared spunlace non-woven fabric has excellent antibacterial property.
In addition, compared with the way of directly adopting the antibacterial fiber, the spunlace non-woven base fabric in this application is directly padded and sized after web-forming and spunlace bonding. On one hand, the operation is simpler and more convenient, and the production cycle is shorter, thus the spunlace non-woven fabric can be mass-produced in a short time to meet the demand. The property of the non-woven fabric as excellent antibacterial and antivirus effects can be ensured, which is of great significance regarding the supply of various medical products during the epidemic when the fabric is applied in the disposable medical products. On the other hand, by padding in the organic copper complex solution, pores inside the spunlace non-woven fabric are uniformly infiltrated, thus the antibacterial effect is uniform, which can effectively prevent substances from precipitating in the pores of the spunlace non-woven fabric after drying.
Further, the fiber includes at least one selected from a group consisting of a natural fiber, an artificial cellulose fiber, an artificial protein fiber, a polyacrylonitrile fiber, and a polyvinyl alcohol fiber.
The molecular structure of the above-mentioned fiber contains free hydroxyl groups, thus formed spunlace non-woven base fabric contains free hydroxyl groups. When the spunlace non-woven base fabric is padded in the organic copper complex solution, complexed copper ions chemically chelate with the cellulose fiber or protein fiber, and the two are firmly combined and not easy be separated from each other during use, thus the spunlace non-woven fabric has excellent and long-lasting antibacterial property.
Further, the fabric obtained after forming a web from fiber contains any one selected from a group consisting of ≥5% by weight of a cotton fiber, or 5-65% by weight of a cellulose fiber, or 5-65% by weight of a protein fiber, or 5-65% by weight of a polyacrylonitrile fiber, or 100% by weight of a polyvinyl alcohol fiber having a low temperature solubility; and the organic copper complex solution is obtained by adding water to a 5.5 wt % initial organic copper complex solution by a volume of 10-30 times more than that of the 5.5 wt % initial organic copper complex solution.
By adopting the above-mentioned technical solution, the copper contained in the spunlace non-woven fabric is finally controlled by controlling the amount of the fiber such as the cotton fiber and cellulose fiber in the fabric obtained after web-formation and the concentration of copper ions in the organic copper complex solution, thereby achieving excellent antibacterial and antivirus effects.
In addition, when the fabric contains 100% by weight of the polyvinyl alcohol fiber being dissolved at the low temperature, it can be dissolved in the low temperature water, which reduces the generation of waste, particularly is of great importance in disposing current medical waste.
Further, the initial organic copper complex solution is prepared by the following steps: preparing a coordination ionic liquid: mixing urea, caprolactam, and acetamide thoroughly, heating, and keep a temperature until the caprolactam and the urea are melted and liquefied thoroughly to obtain the coordination ionic liquid; and
preparing the organic copper complex solution: adding a coordination solid mixture containing sodium chloride, potassium permanganate, sodium peroxide, and copper powder into the coordination ionic liquid under stirring to cause a reaction, cooling, and pouring pure water to obtain an initial organic copper complex solution containing 5.5 wt % copper.
By adopting the above-mentioned technical solution, the organic copper complex solution is used for preparing the spunlace non-woven fabric, and compared with inorganic copper, the organic copper is safer and more reliable, has good compatibility with the environment and a long-lasting antibacterial effect. The copper content contained in the spunlace non-woven fabric can be finally controlled by controlling the concentration of the copper ions in the initial organic copper complex solution and the amount of added water, ensuring excellent antibacterial and antivirus properties.
Further, in the step of preparing the coordination ionic liquid: a ratio of urea:caprolactam:cetamide is in a range of 1:(0.2-0.4):(0.2-0.4) by weight, the constant temperature after mixing urea, caprolactam, and acetamide is in a range of 100-120° C., and the time period of keeping the temperature is in a range of 0.5-1 h.
Further, in the step of preparing the organic copper complex solution: a weight ratio of sodium chloride:potassium permanganate:sodium peroxide:the copper powder is in a range of 1:(1-2):(1-2):(2.5-2.9), and a weight ratio of coordination solid mixture:coordination ionic liquid is in a range of 1:(3-3.5).
In the step of preparing the organic copper complex solution, the copper powder is fully oxidized into monovalent ions chelating with the organic compounds in the coordination ionic liquid to form complexed copper by controlling the weight ratio of the sodium chloride, potassium permanganate, sodium peroxide, and copper powder.
Further, when the fiber includes one or more selected from the group consisting of a polyester fiber, a polyamide fiber, a polyvinyl chloride fiber, and a polypropylene fiber, the spunlace non-woven base fabric is subjected to a step of padding in a chitosan-ascorbic acid solution before being padded and sized. Specifically, the step of padding in a chitosan-ascorbic acid solution comprises padding the spunlace non-woven base fabric in the chitosan-ascorbic acid solution and drying the spunlace non-woven base fabric at a temperature of 150-170° C. for 5-10 min, in which the chitosan-ascorbic acid solution is prepared by adding 5-10 parts by weight of chitosan powder into 25-30 parts by weight of acetic acid and 60-70 parts by weight of water under magnetic stirring until the chitosan powder is dissolved, and adding 3-5 parts by weight of ascorbic acid under stirring thoroughly.
Both the chitosan and ascorbic acid contain free hydroxyl groups, and the chitosan and ascorbic acid penetrate into pores inside the spunlace non-woven base fabric by padding the spunlace non-woven base fabric in the chitosan-ascorbic acid solution, which enhances hydroxyl binding points on the spunlace non-woven base fabric, thereby providing more binding sites for complexed copper ions when the spunlace non-woven base fabric is subsequently padded in the organic copper complex solution. In addition, compared with the divalent copper ion, the covalency of the coordinate bond of the monovalent copper ion is stronger, thus the stability of the coordination complex of the monovalent copper ion is higher than that of the divalent copper ion. In this application, the strong reducibility of the ascorbic acid is used to prevent the monovalent copper ions from being oxidized into divalent copper ions, thereby enhancing the antibacterial property and the persistence of the antibacterial property.
Chitosan has a relative strong attachment property after being dissolved. After being added to the system, it may be firmly attached to the spunlace non-woven base fabric and enhance the bonding between the ascorbic acid and the spunlace non-woven base fabric. The addition of the acetic acid can not only dissolve the chitosan, but also enhance the attachment between the chitosan and spunlace non-woven base fabric, such that the chitosan and ascorbic acid are firmly attached to the spunlace non-woven base fabric which is to be subsequently dried and padded. In addition, the chitosan also has certain antibacterial property and excellent hygroscopicity, which can further enhance the antibacterial property and hygroscopicity of the spunlace non-woven fabric.
Further, the spunlace non-woven base fabric is subjected to a step of soaping after the step of padding in the chitosan-ascorbic acid solution, comprising soaping the spunlace non-woven base fabric after dried in a 5 g/L soaping agent at a soaping temperature of 35-40° C. for 5-10 min, and drying at a drying temperature of 50-60° C.
By adopting the above-mentioned technical solution, the spunlace non-woven base fabric is soaped after being padded in the chitosan-ascorbic acid solution, such that the chitosan and ascorbic acid which are not firmly attached to the spunlace non-woven base fabric can be washed away, preventing the chitosan and ascorbic acid from getting into the organic copper complex solution and chelating with the complexed copper ions during the subsequent process of padding.
At a second aspect, this application provides a Cu-containing non-woven fabric with antibacterial and antiviral properties having a good antibacterial property as well as a certain antivirus property.
Specifically, this application provides the following technical solution: a Cu-containing non-woven fabric is prepared by the method according to the first aspect.
By adopting the above-mentioned technical solution, antibacterial and antivirus properties of the spunlace non-woven fabric are improved while keeping advantages of good air permeability, high hygroscopicity, and low tendency to pill, so that the spunlace non-woven fabric may be widely used.
At a third aspect, this application provides an application of the Cu-containing non-woven fabric with antibacterial and antiviral properties which has an advantage of being widely used.
Specifically, this application provides the following technical solution: an application of the Cu-containing non-woven fabric with antibacterial and antiviral properties as mentioned above in medical and health products.
By adopting the above-mentioned technical solution, the non-woven fabric obtained in this application has excellent antibacterial and antiviral properties, which can be widely used in medical and health produces, such as operating coats, operating cover cloth, medical bandage materials, wound dressings, medical gauze, masks and so on.
In summary, this application has the following beneficial effects.
1. In this application, the spunlace non-woven fabric is padded and sized in the organic copper complex solution so as to use the antibacterial and antivirus effects of the copper element. On one hand, the copper element presents in the form of complexed copper ions between fibers of the spunlace non-woven fabric thereby playing a good antibacterial effect. The spunlace non-woven fabric plays excellent antibacterial and antiviral effects by controlling the concentration of the copper ion on the Cu-containing spunlace non-woven fabric. On the other hand, the organic copper complex solution can not only be coated on the surface of the spunlace non-woven fabric, but also penetrate into pores inside the spunlace non-woven fabric, such that there are copper ions both on the surface and inside the spunlace non-woven fabric especially pores between fibers, thereby playing a good antibacterial effect.
2. Compared with the way of directly adopting the antibacterial fiber, the spunlace non-woven base fabric in this application is directly padded and sized after web-forming and spunlace bonding. On one hand, by padding in the organic copper complex solution, pores inside the spunlace non-woven fabric are uniformly infiltrated, thus the antibacterial effect is uniform, which can effectively prevent substances from precipitating in the pores of the spunlace non-woven fabric after drying. On the other hand, the operation is simpler and more convenient, and the production cycle is shorter, thus the spunlace non-woven fabric can be mass-produced in a short time to meet the demand. The property of the non-woven fabric as excellent antibacterial and antivirus properties can be ensured, which is of great significance regarding the supply of various medical products during the epidemic when the fabric is applied in the disposable medical products.
3. In this application, the fiber used for web-forming includes at least one of the natural fiber, artificial cellulose fiber, artificial protein fiber, polyacrylonitrile fiber, and polyvinyl alcohol fiber. The spunlace non-woven base fabric contains free hydroxyl groups. When the spunlace non-woven base fabric is padded in the organic copper complex solution, complexed copper ions chemically chelate with hydroxyl groups, and the two are firmly combined and not easy to be separated from each other during use, thus the obtained spunlace non-woven fabric has excellent and long-lasting antibacterial property.
This application will be further explained in detail below in combination with examples. These examples are only an explanation of this application, and do not limit the protection scope of this application. It shall be carried out according to conventional conditions or the conditions recommended by the manufacturer if conditions are not specified in the examples.
It should be noted that the spunlace technology can process various kinds of fibers, such as a cotton fiber, a nylon fiber, a polypropylene fiber, a polyester fiber, a viscose fiber and other common fibers. Therefore, the material of the spunlace non-woven fabric obtained in the step of preparing the spunlace non-woven base fabric is not limited, which can be a cellulose fiber such as the viscose fiber, a protein fiber such as a peanut protein fiber, and can also be a fiber selected from a group consisting of a polyester fiber, a polyamide fiber, a polyacrylonitrile fiber, a polyvinyl chloride fiber, a polypropylene fiber, or a polyvinyl alcohol fiber. The Cu-containing spunlace non-woven fabric contains ≥500 ppm copper by controlling the copper content contained in the organic copper complex solution, preferably, 1000-8000 ppm.
For the purpose of forming a chemical chelation between complexed copper ions in an organic copper complex solution and the fiber of the spunlace non-woven fabric, making copper ions difficult to be separated, and making the spunlace non-woven fabric have excellent and long-lasting antibacterial property, in the step of preparing the spunlace non-woven base fabric, the fiber used for web-formation includes any one of a natural fiber or the fiber obtained by wet spinning. Specifically, the fiber includes at least one selected from a group consisting of a natural fiber, an artificial cellulose fiber, an artificial protein fiber, a polyacrylonitrile fiber, and a polyvinyl alcohol fiber. All the above-mentioned fibers contain hydroxyl groups, and the fabric obtained after web-formation contains free hydroxyl groups which can chemically chelate with complexed copper ions when the spunlace non-woven base fabric is padded in the organic copper complex solution, thus the two are firmly combined with each other. The fiber used for web-formation can be the viscose fiber or the peanut protein fiber, or the mixture of the viscose fiber and the protein fiber. Preferably, the fabric obtained after web-formation includes ≥5% by weight of a cotton fiber, or 5-65% by weight of the cellulose fiber, or 5-65% by weight of the protein fiber, or 5-65% by weight of the polyacrylonitrile fiber, or 100% by weight of the polyvinyl alcohol fiber being dissolved at a low temperature. Any one of the above-mentioned solutions can be adopted, but this application is not limited thereto. When the fiber is a mixture of the above-mentioned hydroxyl-containing fiber and non-hydroxyl-containing fiber, it is only necessary that the sum of the hydroxyl-containing fibers in the fabric after web-formation can reach the minimum amount. For example, if the cotton fiber, viscose fiber, and polyester fiber are adopted, it is only necessary to ensure that the sum of the cotton fiber and viscose fiber in the fabric is ≥5 wt %. If the viscose fiber, polyacrylonitrile fiber, and polyester fiber are adopted, it is only necessary to ensure that the sum of the viscose fiber and polyacrylonitrile fiber is in a range of 5-65 wt %. The copper content contained in the spunlace nonwoven fabric is finally controlled by controlling the amount of the fiber in the fabric and the copper content in the organic copper complex solution.
The above-mentioned polyvinyl alcohol fiber being dissolved at the low temperature can be directly dissolved in the water with a low temperature of 20-98° C.
When the fiber used for web-formation does not contain hydroxyl groups, for example, the fiber includes one or more selected from a group consisting of a polyester fiber, a polyamide fiber, a polyvinyl chloride fiber, and a polypropylene fiber, the spunlace nonwoven fabric is padded in a chitosan-ascorbic acid solution before being padded and sized so as to increase the bonding between the complexed copper ions and spunlace nonwoven fabric. Both the chitosan and ascorbic acid contain free hydroxyl groups, and by using the attachment property of the chitosan and adding acetic acid into the chitosan ascorbic acid solution, the chitosan and ascorbic acid are more firmly attached to the spunlace non-woven base fabric which is chemically chelated with copper ions in the organic copper complex solution, thereby enhancing the bonding between organic copper and spunlace non-woven fabric.
This application will be further explained in detail below in combination with preparation examples, examples, and comparation examples.
Preparation Examples 1-5 are examples for preparing the organic copper complex solution.
A method for preparing an organic copper complex solution included the following steps:
Step S1. preparing a coordination ionic liquid: mixing urea, caprolactam, and acetamide thoroughly according to a ratio of 1:0.2:0.2 by weight, heating to a temperature of 100° C. and keeping the temperature for 1 h until the caprolactam and the urea were melted and liquefied thoroughly to obtain the coordination ionic liquid; and
Step S2. preparing an organic copper complex solution: weighting sodium chloride, potassium permanganate, sodium peroxide, and copper powder according to a ratio of 1:1:1:2.5 by weight, mixing them to obtain a coordination solid mixture, adding the coordination solid mixture into the coordination ionic liquid and stirring thoroughly, a ratio of the coordination solid mixture and the coordination ionic liquid being 1:3 by weight, the copper powder being fully oxidized into monovalent ions and forming coordination ions with organic compounds in the coordination ionic liquid, adding pure water after being cooled to obtain an initial organic copper complex solution containing 5.5 wt % copper with no precipitation or discoloration occurred after 3 days, and adding water into the initial organic copper complex solution by a volume of 10 times more than the initial organic copper complex solution so as to obtain the organic copper complex solution.
A method for preparing an organic copper complex solution included the following steps:
Step S1. preparing a coordination ionic liquid: mixing urea, caprolactam, and acetamide thoroughly according to a ratio of 1:0.3:0.4 by weight, heating to a temperature of 110° C. and keeping the temperature for 0.5 h until the caprolactam and the urea were melted and liquefied thoroughly to obtain the coordination ionic liquid; and Step S2. preparing an organic copper complex solution: weighting sodium chloride, potassium permanganate, sodium peroxide, and copper powder according to a ratio of 1:2:1:2.9 by weight, mixing them to obtain a coordination solid mixture, adding the coordination solid mixture into the coordination ionic liquid and stirring thoroughly, a ratio of the coordination solid mixture and the coordination ionic liquid being 1:3.5 by weight, the copper powder being fully oxidized into monovalent ions and forming coordination ions with organic compounds in the coordination ionic liquid, adding pure water after being cooled to obtain an initial organic copper complex solution containing 5.5 wt % copper with no precipitation or discoloration occurred after 3 days, and adding water into the initial organic copper complex solution by a volume of 20 times more than the initial organic copper complex solution so as to obtain the organic copper complex solution.
A method for preparing an organic copper complex solution included the following steps:
Step S1. preparing a coordination ionic liquid: mixing urea, caprolactam, and acetamide thoroughly according to a ratio of 1:0.4:0.4 by weight, heating to a temperature of 120° C. and keeping the temperature for 1 h until the caprolactam and the urea were melted and liquefied thoroughly to obtain the coordination ionic liquid; and
Step S2. preparing an organic copper complex solution: weighting sodium chloride, potassium permanganate, sodium peroxide, and copper powder according to a ratio of 1:2:2:2.9 by weight, mixing them to obtain a coordination solid mixture, adding the coordination solid mixture into the coordination ionic liquid and stirring thoroughly, a ratio of the coordination solid mixture and the coordination ionic liquid being 1:3.5 by weight, the copper powder being fully oxidized into monovalent ions and forming coordination ions with organic compounds in the coordination ionic liquid, adding pure water after being cooled to obtain an initial organic copper complex solution containing 5.5 wt % copper with no precipitation or discoloration occurred after 3 days, and adding water with a volume of 30 times than the initial organic copper complex solution into the initial organic copper complex solution so as to obtain the organic copper complex solution.
A method for preparing an organic copper complex solution was carried out according to the method in Preparation Example 2, except that water with a volume of 15 times more than the initial organic copper complex solution was added so as to obtain the organic copper complex solution.
A method for preparing an organic copper complex solution was carried out according to the method in Preparation Example 2, except that water with a volume of 25 times more than the initial organic copper complex solution was added so as to obtain the organic copper complex solution.
Preparation Examples 6-10 are examples for preparing the chitosan-ascorbic acid solution.
A method for preparing a chitosan-ascorbic acid solution included the following steps:
adding 5 kg chitosan powder into 25 kg acetic acid and 60 kg water under magnetic stirring until the chitosan powder was dissolved, then adding 3 kg ascorbic acid, and stirring thoroughly.
A method for preparing a chitosan-ascorbic acid solution included the following steps: adding 8 kg chitosan powder into 28 kg acetic acid and 65 kg water under magnetic stirring until the chitosan powder was dissolved, then adding 4 kg ascorbic acid, and stirring thoroughly.
A method for preparing a chitosan-ascorbic acid solution included the following steps:
adding 10 kg chitosan powder into 30 kg acetic acid and 70 kg water under magnetic stirring until the chitosan powder was dissolved, then adding 5 kg ascorbic acid, and stirring thoroughly.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties included the following steps:
preparing a spunlace non-woven base fabric: forming a web from a mixed fiber of a viscose fiber and a polyester fiber, pre-wetting the web, and spunlacing the web to obtain the spunlace non-woven base fabric, and the fabric obtained after forming the web containing 5 wt % viscose fiber;
padding and sizing: padding and sizing the spunlace non-woven base fabric in an organic copper complex solution through a sizing machine to obtain a Cu-containing spunlace non-woven fabric, wherein the organic copper complex solution in the sizing machine was prepared from Preparation Example 2; and
drying at a drying temperature of 90° C. and winding the Cu-containing spunlace non-woven fabric after being padded and sized.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties included the following steps:
preparing a spunlace non-woven base fabric: forming a web from a mixed fiber of a viscose fiber, a polyacrylonitrile fiber, and a polyester fiber, pre-wetting the web, and spunlacing the web to obtain the spunlace non-woven base fabric, and the sum of the viscose fiber and the polyester fiber after web-forming being 65 wt %;
padding and sizing: padding and sizing the spunlace non-woven base fabric in an organic copper complex solution through a sizing machine to obtain a Cu-containing spunlace non-woven fabric, wherein the organic copper complex solution in the sizing machine was prepared from Preparation Example 1; and
drying at a drying temperature of 100° C. and winding the Cu-containing spunlace non-woven fabric after being padded and sized.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties included the following steps:
preparing a spunlace non-woven base fabric: forming a web from a mixed fiber of a cotton fiber and a polyester fiber, pre-wetting the web, and spunlacing the web to obtain the spunlace non-woven base fabric, and the fabric obtained after web-forming containing 5 wt % cotton fiber;
padding and sizing: padding and sizing the spunlace non-woven base fabric in an organic copper complex solution through a sizing machine to obtain a Cu-containing spunlace non-woven fabric, wherein the organic copper complex solution in the sizing machine was prepared from Preparation Example 5; and
drying at a drying temperature of 100° C. and winding the Cu-containing spunlace non-woven fabric after being padded and sized.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties was carried out according the method in Example 2 except that,
preparing the spunlace non-woven base fabric: web-forming a web from a mixed fiber of a soybean fiber and a polyester fiber, pre-wetting the web, and spunlacing the web to obtain the spunlace non-woven base fabric, and the fabric obtained after web-forming containing 20 wt % soybean fiber; and
the organic copper complex solution in the sizing machine was prepared from Preparation Example 3.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties was carried out according the method in Example 2 except that,
preparing the spunlace non-woven base fabric: forming a web from a polyvinyl alcohol fiber having a low-temperature water solubility, pre-wetting the web, and spunlacing the web to obtain the spunlace non-woven base fabric, wherein the polyvinyl alcohol fiber having a low-temperature water solubility can be directly dissolved in water at a temperature of 20° C.; and
the organic copper complex solution in the sizing machine was prepared from Preparation Example 4.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties included the following steps:
preparing a spunlace non-woven base fabric: forming a web from a polypropylene fiber, pre-wetting the web, and spunlacing the web to obtain the spunlace non-woven base fabric;
padding in an chitosan-ascorbic acid solution: padding the spunlace non-woven base fabric in the chitosan-ascorbic acid solution through a sizing machine, then drying at a temperature of 150° C. for 10 min, wherein the chitosan-ascorbic acid solution in the sizing machine was prepared from Preparation Example 6;
soaping: soaping the dried spunlace non-woven base fabricin a 5 g/L soaping agent at a soaping temperature of 35° C. for 10 min, and drying at a drying temperature of 50° C., wherein the soaping agent was purchased from Dongguan Chain Spinning New Material Technology Co. Ltd., the brand was chain spinning Texchain, and the model was 605;
padding and sizing: padding and sizing the soaped spunlace non-woven base fabric in an organic copper complex solution through a sizing machine to obtain a Cu-containing spunlace non-woven fabric, wherein the organic copper complex solution in the sizing machine was prepared from Preparation Example 1; and
drying at a drying temperature of 100° C. and winding the Cu-containing spunlace non-woven fabric after being padded and sized.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties included the following steps:
preparing a spunlace non-woven base fabric: forming a web from a polyamide fiber, pre-wetting the web, and spunlacing the web to obtain the spunlace non-woven base fabric;
padding in an chitosan-ascorbic acid solution: padding the spunlace non-woven base fabric in the chitosan-ascorbic acid solution through a sizing machine, then drying at a temperature of 160° C. for 8 min, wherein the chitosan-ascorbic acid solution in the sizing machine was prepared from Preparation Example 7;
soaping: soaping the dried spunlace non-woven base fabric in a 5 g/L soaping agent at a soaping temperature of 40° C. for 5 min, and drying at a drying temperature of 55° C., wherein the soaping agent was purchased from Dongguan Chain Spinning New Material Technology Co. Ltd., the brand was chain spinning Texchain, and the model was 605;
padding and sizing: padding and sizing the soaped spunlace non-woven base fabric in an organic copper complex solution through a sizing machine to obtain a Cu-containing spunlace non-woven fabric, wherein the organic copper complex solution in the sizing machine was prepared from Preparation Example 2; and
drying at a drying temperature of 100° C. and winding the Cu-containing spunlace non-woven fabric after being padded and sized.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties included the following steps:
preparing a spunlace non-woven base fabric: web-forming a web from a polyvinyl chloride fiber, pre-wetting the web, and spunlacing the web to obtain the spunlace non-woven base fabric;
padding in an chitosan-ascorbic acid solution: padding the spunlace non-woven base fabric in the chitosan-ascorbic acid solution through a sizing machine, then drying at a temperature of 170° C. for 5 min, wherein the chitosan-ascorbic acid solution in the sizing machine was prepared from Preparation Example 8;
soaping: soaping the dried spunlace non-woven base fabric after in a 5 g/L soaping agent at a soaping temperature of 40° C. for 5 min, and drying at a drying temperature of 60° C., wherein the soaping agent was purchased from Dongguan Chain Spinning New Material Technology Co. Ltd., the brand was chain spinning Texchain, and the model was 605;
padding and sizing: padding and sizing the soaped spunlace non-woven base fabric in an organic copper complex solution through a sizing machine to obtain a Cu-containing spunlace non-woven fabric, wherein the organic copper complex solution in the sizing machine was prepared from Preparation Example 3; and
drying at a drying temperature of 100° C. and winding the Cu-containing spunlace non-woven fabric after padded and sized.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties was carried out according the method in Example 2 except that, in the step of padding and sizing, when preparing the organic copper complex solution in the sizing machine, the initial organic copper complex solution was added into pure water with a volume of 12 times more than the initial organic copper complex solution, and the rest was the same as Preparation Example 2.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties was carried out according the method in Example 2 except that, in the step of padding and sizing, when preparing the organic copper complex solution in the sizing machine, the initial organic copper complex solution was added into pure water with a volume of 25 times more than the initial organic copper complex solution, and the rest was the same as Preparation Example 2.
A method for preparing a Cu-containing non-woven fabric with antibacterial and antiviral properties was carried out according the method in Example 2 except that, in the step of padding and sizing, the solution in the sizing machine was not the organic copper complex solution but a 3 mol/L copper chloride solution.
Property Test
1. Antibacterial Property Test
Antibacterial properties of spunlace non-woven base fabrics obtained from examples 1-8 were determined according to AATCC 100-2012. The test sample was a circular swatch with a diameter of 4.8 cm, and 4 parallel tests were carried out with an average value being taken. The test bacteria was Methicillin-resistant Staphylococcus aureus ATCC 33591, and the volume of the inoculum was 1 mL. Results of the test were shown as Table 1.
Staphylococcus
aureus ATCC 33591
Similarly, the above-mentioned antibacterial property test was carried out for spunlace non-woven base fabrics obtained from comparation examples 1-3, and results were shown as table 2.
Staphylococcus
aureus ATCC 33591
It can be seen from table 1 that antibacterial properties of spunlace non-woven fabrics prepared by the method of this application were excellent, especially for Methicillin-resistant Staphylococcus aureus with strong toxicity and drug resistance. In this application, adding water with a volume of 10-30 times than an initial organic copper complex solution into the initial organic copper complex solution with a weight percentage of 5.5 wt %, and controlling fiber materials used for web-formation, the concentration of copper ions on the spunlace non-woven fabric was controlled to be in a range of 500-8000 ppm, which played an excellent antibacterial effect. Combining with comparation example 3 and example 2, it can be seen that the antibacterial property was greatly improved by using organic copper complex ions in this application than by directly adding inorganic copper. Referring to comparation examples 1-2 and example 2, it can be seen that the antibacterial effect was greatly reduced when the concentration of copper ions in the organic copper complex solution was very low, and when the concentration of copper ions was very high, the antibacterial property kept unchanged while the cost was increased, meanwhile the copper with a high content was harmful for the human body.
In addition, when spunlace non-woven fabrics containing hydroxyl groups in examples 1-5 were directly padded in the organic copper complex solution, the antibacterial effect thereof was excellent. Meanwhile, because the raw material of the spunlace non-woven fabric was polyester which was the synthetic fiber and did not contain cellulose, it should be padded in the chitosan-ascorbic acid solution in advance and then padded in the organic complex copper solution, and the obtained spunlace non-woven fabric also had excellent antibacterial property.
2. Persistence Property Test
After respectively washing spunlace non-woven base fabrics for 50, 100, and 200 times, antibacterial properties of spunlace non-woven base fabrics obtained from examples 1 and 7 and comparation examples 1 and 3 were determined according to AATCC 100-2012. The test sample was a circular swatch with a diameter of 4.8 cm, the test bacteria was Methicillin-resistant Staphylococcus aureus ATCC 33591, and the volume of the inoculum was 1 mL. Furthermore, the copper content on spunlace non-woven fabrics was tested to determine the loss of copper content. Results of the test were shown as Table 3.
It can be seen from table 3 that after washing spunlace non-woven fabrics for 50, 100 and 200 times, the antibacterial effect of spunlace non-woven fabrics on methicillin-resistant Staphylococcus aureus in this application did not significantly change and had excellent persistence property.
3. Antivirus Property Test
The antivirus property test was performed on the spunlace non-woven fabric prepared in example 2, specifically, Murine norovirus s99 was used in place of human norovirus in inactivation residual activity test on human skin, in which the skin was obtained as follow.
Skin substrate. Skin was obtained from Tissue Solutions Limited, UK. The sample was used under licence. Cat #T-SKN-CUSTOM. Lot #SKINMD10413C. Was delivered under dry ice, next day delivery and stored at 8° C. Caucasian, thigh/hip. Female 46 years. BMI 24. Freeze date: 01/04/13. The Skin was thawed and dissected to remove subcutaneous tissue immediately before use.
Test Steps:
i) Virus stock: MNV 260315.17, stored at −80° C. Thawed immediately before use.
ii) The action of the wet wipe on skin (approximately 1.0×1.0 cm patches, freshly prepared), N=5 in a separate sterile plastic petri dish at 3 minute intervals, was simulated by using a standard wipe motion: The skin was held in one corner by sterile forceps and three strokes of the wipe were made along one axis of the skin patch covering the surface of the skin and then three strokes performed at 90°. This was then repeated. The duration of this was 30 seconds.
iii) After 4 hours incubation at room temperature, 50 μl of virus suspension was inoculated onto the surface of the patch for 1 minute.
iv) The skin patch was transferred to 2.0 ml cold cell culture medium (Dulbecco's modified Eagle's medium (DMEM)+5.0% V/V Foetal bovine serum)+1.0 g sterile glass beads and vortexed for 20 seconds. The recovery medium was filtered through a 0.45 μm filter to remove contaminating bacteria and stored at −20° C. overnight. A 0.1 ml volume was neutralized by gel filtration (Microspin S-400 HR column) and the eluent (void volume) was serially 10-fold diluted for TCID50 assay.
where Σn is the sum of the proportions of wells infected from the 10−1 to the 10−6 dilution of the virus.
Results of the test were shown as Table 4.
According to the protocol described against Murine norovirus s99 Berlin strain/RAW cells a surrogate for human norovirus, Cu-containing non-woven fabric achieved the following performance in vitro when compared to a non-woven fabric control:
Cu-containing non-woven fabric upon contact with the virus for 60 seconds, 4 hours after application onto to human skin, achieved a mean percent reduction of 57.32% in virus bioactivity compared to the non-woven fabric control. This product when applied (as wiping) to skin therefore shows a residual affect after 4 hours.
In summary, the spunlace non-woven fabric prepared by the method in this application has antibacterial and antivirus properties, which can be widely used in medical and health, domestic decoration, clothing, industry, agriculture and other fields, especially in medical and health products such as masks and operating coats.
These embodiments are only an explanation of this invention, and do not limit the protection scope of this invention. Those skilled in the art can make modifications without creative contribution to this embodiment after reading this specification, and it is protected by the patent law as long as it is within the scope of the claims of this invention.
| Number | Date | Country | Kind |
|---|---|---|---|
| 202010427848.8 | May 2020 | CN | national |
