WO2021232870A1 - Non-tissé antimicrobien et antiviral contenant du cuivre et procédé de préparation de celui-ci - Google Patents
Non-tissé antimicrobien et antiviral contenant du cuivre et procédé de préparation de celui-ci Download PDFInfo
- Publication number
- WO2021232870A1 WO2021232870A1 PCT/CN2021/077409 CN2021077409W WO2021232870A1 WO 2021232870 A1 WO2021232870 A1 WO 2021232870A1 CN 2021077409 W CN2021077409 W CN 2021077409W WO 2021232870 A1 WO2021232870 A1 WO 2021232870A1
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- WO
- WIPO (PCT)
- Prior art keywords
- copper
- fiber
- spunlace
- woven fabric
- solution
- Prior art date
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 187
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 175
- 239000010949 copper Substances 0.000 title claims abstract description 175
- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 130
- 238000002360 preparation method Methods 0.000 title claims abstract description 67
- 230000000840 anti-viral effect Effects 0.000 title claims abstract description 51
- 230000000845 anti-microbial effect Effects 0.000 title abstract 5
- 239000000835 fiber Substances 0.000 claims abstract description 200
- 239000004744 fabric Substances 0.000 claims abstract description 132
- 238000004513 sizing Methods 0.000 claims abstract description 60
- 238000000034 method Methods 0.000 claims abstract description 48
- 239000002657 fibrous material Substances 0.000 claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 18
- 230000002787 reinforcement Effects 0.000 claims abstract description 11
- 238000009736 wetting Methods 0.000 claims abstract description 10
- 230000000844 anti-bacterial effect Effects 0.000 claims description 83
- 229960005070 ascorbic acid Drugs 0.000 claims description 44
- 239000011668 ascorbic acid Substances 0.000 claims description 44
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 28
- 239000002608 ionic liquid Substances 0.000 claims description 26
- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 claims description 24
- 229920001661 Chitosan Polymers 0.000 claims description 23
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 21
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 19
- 235000010323 ascorbic acid Nutrition 0.000 claims description 15
- DLFVBJFMPXGRIB-UHFFFAOYSA-N Acetamide Chemical compound CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 14
- 229920000728 polyester Polymers 0.000 claims description 13
- 239000004202 carbamide Substances 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 11
- 108090000623 proteins and genes Proteins 0.000 claims description 11
- 102000004169 proteins and genes Human genes 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 11
- 229920000742 Cotton Polymers 0.000 claims description 10
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 10
- 239000008247 solid mixture Substances 0.000 claims description 10
- -1 polyethylene Polymers 0.000 claims description 8
- 239000012286 potassium permanganate Substances 0.000 claims description 8
- PFUVRDFDKPNGAV-UHFFFAOYSA-N sodium peroxide Chemical compound [Na+].[Na+].[O-][O-] PFUVRDFDKPNGAV-UHFFFAOYSA-N 0.000 claims description 8
- 229920003043 Cellulose fiber Polymers 0.000 claims description 7
- 239000004743 Polypropylene Substances 0.000 claims description 7
- 239000003795 chemical substances by application Substances 0.000 claims description 7
- 229920001155 polypropylene Polymers 0.000 claims description 7
- 239000011780 sodium chloride Substances 0.000 claims description 7
- 239000004952 Polyamide Substances 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 150000004699 copper complex Chemical class 0.000 claims description 5
- 229920002647 polyamide Polymers 0.000 claims description 5
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 5
- 239000004800 polyvinyl chloride Substances 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims 1
- 239000004698 Polyethylene Substances 0.000 claims 1
- 229920000573 polyethylene Polymers 0.000 claims 1
- 238000001035 drying Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 238000004804 winding Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 118
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 22
- 229910001431 copper ion Inorganic materials 0.000 description 21
- 238000012360 testing method Methods 0.000 description 17
- 229920000297 Rayon Polymers 0.000 description 15
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 14
- 241000700605 Viruses Species 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 9
- 239000000463 material Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 206010033675 panniculitis Diseases 0.000 description 6
- 210000004304 subcutaneous tissue Anatomy 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 5
- RJQXTJLFIWVMTO-TYNCELHUSA-N Methicillin Chemical compound COC1=CC=CC(OC)=C1C(=O)N[C@@H]1C(=O)N2[C@@H](C(O)=O)C(C)(C)S[C@@H]21 RJQXTJLFIWVMTO-TYNCELHUSA-N 0.000 description 4
- 241000191967 Staphylococcus aureus Species 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000002155 anti-virotic effect Effects 0.000 description 4
- 230000009920 chelation Effects 0.000 description 4
- 229960003085 meticillin Drugs 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 239000002964 rayon Substances 0.000 description 4
- 235000017060 Arachis glabrata Nutrition 0.000 description 3
- 244000105624 Arachis hypogaea Species 0.000 description 3
- 235000010777 Arachis hypogaea Nutrition 0.000 description 3
- 235000018262 Arachis monticola Nutrition 0.000 description 3
- 239000006144 Dulbecco’s modified Eagle's medium Substances 0.000 description 3
- 241001263478 Norovirus Species 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000002845 discoloration Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000011081 inoculation Methods 0.000 description 3
- 239000002609 medium Substances 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 235000020232 peanut Nutrition 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
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- 239000004753 textile Substances 0.000 description 3
- 244000068988 Glycine max Species 0.000 description 2
- 235000010469 Glycine max Nutrition 0.000 description 2
- 241001105894 Murine norovirus Species 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229920002678 cellulose Polymers 0.000 description 2
- 239000001913 cellulose Substances 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- 150000001879 copper Chemical class 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000002759 woven fabric Substances 0.000 description 2
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 1
- 108091003079 Bovine Serum Albumin Proteins 0.000 description 1
- 241000282465 Canis Species 0.000 description 1
- 208000035473 Communicable disease Diseases 0.000 description 1
- 208000035240 Disease Resistance Diseases 0.000 description 1
- 241000712431 Influenza A virus Species 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000006143 cell culture medium Substances 0.000 description 1
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012091 fetal bovine serum Substances 0.000 description 1
- 238000002523 gelfiltration Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 238000011534 incubation Methods 0.000 description 1
- 210000001985 kidney epithelial cell Anatomy 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- 239000002906 medical waste Substances 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
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- 231100000331 toxic Toxicity 0.000 description 1
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- 238000013022 venting Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- 238000002166 wet spinning Methods 0.000 description 1
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Definitions
- This application relates to the technical field of non-woven fabrics, and more specifically, it relates to a copper-containing antibacterial and antiviral non-woven fabric and a preparation method thereof.
- Spunlace non-woven fabrics are fabrics in which high-pressure fine water jets are sprayed onto one or more layers of fiber webs to entangle the fibers so that the webs can be reinforced and have a certain strength. Because of its advantages of high strength, low fuzz, high moisture absorption and good air permeability, spunlace nonwovens have become one of the fastest technological advancements in the nonwovens industry in recent years, and are widely used in medical and sanitary nonwovens. Fabrics, non-woven fabrics for home decoration, non-woven fabrics for clothing, non-woven fabrics for industrial use, non-woven fabrics for agricultural use, etc. In particular, in recent years, while the demand for medical and health non-woven fabrics has greatly increased, higher requirements have been placed on its antibacterial and antiviral properties.
- non-woven fabrics are conducive to the adhesion of microorganisms due to their porous shape and the chemical structure of polymer compounds. Therefore, the research and development of antibacterial functions of spunlace non-woven fabrics is of great significance.
- this application provides a method for preparing copper-containing antibacterial and antiviral non-woven fabrics, which has good antibacterial properties and a certain degree of antiviral spunlace.
- the woven fabric has the advantages of simple preparation method, easy realization of industrialization, and simple process.
- this application provides the following technical solution: a method for preparing a copper-containing antibacterial and antiviral non-woven fabric, including the following steps:
- the fiber material is successively subjected to fiber web formation, pre-wetting, and spunlace reinforcement to obtain a spunlace fiber fabric base fabric;
- the spunlace fiber cloth base fabric is padding sizing in an organic complex copper solution to obtain a copper-containing spunlace non-woven fabric, and the copper content of the copper-containing spunlace non-woven fabric is ⁇ 500ppm;
- the copper-containing spunlace non-woven fabric obtained after padding and sizing is dried and wound.
- the copper element has a strong bactericidal function and a certain antiviral effect.
- the spunlace non-woven fabric is padding sizing in the organic complex copper solution.
- the organic complex copper solution Not only can be coated on the surface of the spunlace non-woven fabric, but also can penetrate into the internal voids of the spunlace non-woven fabric, making the interior of the spunlace non-woven fabric, especially the voids between the fibers and the surface of the spunlace non-woven fabric All have copper ions, which can play a better antibacterial effect.
- the copper element exists in the form of copper ions between the fibers of the spunlace non-woven fabric, and the antibacterial function is more significant, especially the copper-containing spunlace
- the control of the copper ion concentration on the non-woven fabric makes the final spunlace non-woven fabric have excellent antibacterial and antiviral effects.
- the fibrous material fibers are first formed into a web, then pre-wet, and then reinforced by hydroentanglement. Under the action of hydroentanglement, the fiber web moves, intersperses, entangles, and entangles among the fibers. , Forming countless soft entanglement points, consolidating the fiber web to obtain the spunlace fiber cloth base fabric.
- the pre-wetting operation compacts the fluffy fiber web, venting the air in the fiber web, so that the fiber web can enter the spunlace area.
- the spunlace non-woven fabric in the present application is directly padding sizing after fiber formation and spunlace reinforcement during the production process.
- the operation is more simple and convenient, and the process cycle is more convenient. Shorter, large-scale production of spunlace non-woven fabrics in a short period of time, to meet the supply, and can meet the performance of non-woven fabrics, and has excellent antibacterial and antiviral properties. It can be used in disposable medical supplies.
- padding through the organic complex copper solution makes the gaps and areas of the spunlace non-woven fabric evenly infiltrated, and the antibacterial effect is uniform, which can effectively avoid Precipitation of substances in the holes of the spunlace non-woven fabric after drying.
- the fiber material includes at least one of natural fiber, rayon fiber, rayon protein fiber, polyacrylonitrile fiber, and polyvinyl alcohol fiber.
- the molecular structure of the fiber material contains open hydroxyl groups
- the formed spunlace fiber cloth base cloth contains open hydroxyl groups.
- the fabric obtained after the step of forming the fiber material fiber into the web contains ⁇ 5% cotton fiber, or 5-65% cellulose fiber, or 5-65% protein fiber, or 5-65% poly Acrylonitrile fiber, or 100% low melting point polyvinyl alcohol fiber;
- the organic complex copper solution is obtained by adding 5.5 wt% of the initial organic complex copper solution to 10-30 volume multiples of water.
- the fabric when the fabric is 100% low-melting point polyvinyl alcohol fiber, it can be dissolved in low-temperature water, which reduces waste generation, especially for the current medical waste treatment.
- the initial organic complexed copper solution is prepared according to the following method:
- Preparation of organic complex copper solution add the coordination solid mixture including sodium chloride, potassium permanganate, sodium peroxide and copper powder to the coordination ionic liquid, stir uniformly, react, and pour into pure water after cooling to obtain the copper content It is 5.5wt% of the initial organic copper complex solution.
- the organic complex copper solution is used in the spunlace non-woven fabric in this application.
- organic copper is safer and more reliable, has good environmental compatibility, and has good compatibility. Its antibacterial effect lasts for a long time, and the copper content on the final spunlace non-woven fabric can be controlled by the copper ion concentration in the initial organic complexed copper solution and the amount of water added, and finally has excellent antibacterial and antiviral properties.
- the application is further set as follows: in the step of preparing the coordination ionic liquid, the mixing weight ratio of urea, caprolactam and acetamide is 1: (0.2-0.4): (0.2-0.4), and the heating temperature after uniform mixing is 100-120°C, The holding time is 0.5-1h.
- the application is further set as follows: in the step of preparing the organic complex copper solution: the mixing weight ratio of sodium chloride, potassium permanganate, sodium peroxide and copper powder is 1: (1-2): (1-2): ( 2.5-2.9), the mixing weight ratio of the coordination solid mixture and the coordination ionic liquid is 1: (3-3.5).
- the application is further configured as follows: when the fiber material is one or more of polyester fiber, polyamide fiber, polyvinyl chloride fiber, and polypropylene fiber, the spunlace fiber cloth base fabric is also shelled before padding and sizing.
- the dipping step of the glycan-ascorbic acid solution is as follows: the spunlace fiber cloth base cloth is dipped in the chitosan-ascorbic acid solution, and then dried at 150-170°C for 5-10min, the chitosan-ascorbic acid solution
- the preparation method is as follows: add 5-10 parts of chitosan powder to 25-30 parts of acetic acid and 60-70 parts of water, magnetically stir until the chitosan is dissolved, then add 3-5 parts of ascorbic acid, and stir evenly.
- the molecular structures of chitosan and ascorbic acid both have open hydroxyl groups.
- the spunlace fiber cloth base fabric is first dipped in a chitosan-ascorbic acid solution, and the chitosan and ascorbic acid are immersed in the spunlace fiber cloth.
- the hydroxyl binding points on the reinforced spunlace fiber cloth base fabric will have more binding sites with the complex copper ions during the subsequent padding in the organic complex copper solution.
- the coordination bond of monovalent copper is more covalent, so the stability of monovalent copper complexes is stronger than that of divalent copper complexes.
- the strong ascorbic acid is used in this application. Reducing, adding ascorbic acid can inhibit the oxidation of monovalent copper to divalent copper, thereby enhancing the antibacterial performance and the durability of antibacterial functions.
- Chitosan is also added to the system, and the dissolved chitosan has a strong adsorption capacity. Chitosan can be more firmly attached between the spunlace fiber cloth base cloth, and it can also improve the ascorbic acid and spunlace fiber cloth. The bonding strength between the base fabrics.
- the addition of acetic acid can dissolve chitosan on the one hand, and on the other hand, it can also enhance the adsorption between chitosan and the spunlace fiber fabric, so that chitosan and ascorbic acid can be more firmly adsorbed on the spunlace fiber fabric. After drying, the chitosan also has certain antibacterial properties and excellent moisture absorption properties, which can further enhance the antibacterial and moisture absorption properties of the spunlace fiber cloth.
- the application is further set as follows: the spunlace fiber cloth base cloth is subjected to a soaping step after the chitosan-ascorbic acid solution padding step, and the specific operation is: the dried spunlace fiber cloth base cloth is soaped at 5g/L Medium soaping 5-10min, soaping temperature is 35-40°C, and then drying at 50-60°C.
- the spunlace fiber cloth base fabric after the chitosan-ascorbic acid solution is soaked can be soaped, which can remove the weakly bonded chitosan and ascorbic acid on the spunlace fiber cloth base fabric and prevent subsequent soaking.
- chitosan and ascorbic acid enter the organic complexed copper solution and complex with complexed copper ions.
- the present application provides a copper-containing antibacterial and antiviral non-woven fabric, which has the advantages of good antibacterial properties and certain antiviral properties.
- this application provides the following technical solution: a copper-containing antibacterial and antiviral non-woven fabric prepared by the preparation method according to the first aspect described above.
- the spunlace nonwoven fabric prepared by the above method has improved antibacterial and antiviral properties on the basis of maintaining excellent air permeability, high moisture absorption and low fluffing of the spunlace nonwoven fabric.
- the obtained spunlace non-woven fabric has excellent antibacterial and antiviral properties, and has a wide range of applications.
- this application provides an application of a copper-containing antibacterial and antiviral non-woven fabric, which has the advantage of being widely used.
- this application provides the following technical solution: an application of the above-mentioned copper-containing antibacterial and antiviral non-woven fabric in medical and sanitary products.
- the non-woven fabric obtained in this application has excellent antibacterial and disease resistance performance, and has a wide range of products in medical and sanitary products such as surgical gowns, surgical masks, medical dressing materials, wound dressings, medical gauze, and masks. Applications.
- the spunlace non-woven fabric is padding sizing in the organic complex copper solution.
- the copper element is present in the spunlace in the form of complexed copper ions.
- the antibacterial function between the fibers of the woven fabric is more significant, especially by controlling the concentration of copper ions on the spunlace non-woven fabric, which has an antibacterial and antiviral effect.
- the organic complex copper solution can not only be coated on the spunlace
- the surface of the non-woven fabric can penetrate into the internal voids of the spunlace non-woven fabric, so that the interior of the spunlace non-woven fabric, especially the voids between the fibers and the surface of the spunlace non-woven fabric, have copper ions, which can Play a better antibacterial effect;
- the spunlace non-woven fabric in the present application is directly padding sizing after fiber formation and spunlace reinforcement during the production process.
- the padding makes the gaps and areas of the spunlace non-woven fabric evenly infiltrated, and the antibacterial effect is uniform, which can effectively avoid the precipitation of substances in the spunlace non-woven fabric holes after drying; on the other hand, the operation is more simple and convenient.
- the process cycle is shorter, and the spunlace non-woven fabric can be mass-produced in a short time to meet the supply, and can meet the performance of the non-woven fabric, and has excellent antibacterial and antiviral properties. It can be used in disposable medical products. The demand and supply of various medical supplies during the epidemic is of great significance;
- the fiber material used for fiber web formation in this application includes at least one of natural fiber, rayon fiber, rayon fiber, polyacrylonitrile fiber, and polyvinyl alcohol fiber, so that the spunlace fiber cloth base fabric contains The open hydroxyl group will form a chemical chelation between the copper complex and the hydroxyl group during subsequent padding in the organic complex copper solution. The two are firmly combined and will not easily fall off during use. The resulting spunlace fiber cloth is antibacterial and durable. Excellent performance.
- the spunlace process can process various fibers, such as cotton fiber, nylon fiber, polypropylene fiber, polyester fiber or viscose fiber and other common fibers. Therefore, in the preparation step of the spunlace non-woven fabric base fabric in this application
- the material of the obtained spunlace non-woven fabric is not limited.
- cellulose fiber such as viscose fiber, etc.
- protein fiber such as peanut protein fiber, etc.
- polyester fiber polyamide fiber ( Nylon/nylon), polyacrylonitrile fiber (acrylic), polyvinyl chloride fiber (chlorinated fiber), polypropylene fiber (polypropylene) or polyvinyl alcohol fiber (Villen), control water by controlling the copper content in the organic complex copper solution
- the content of copper on the barbed fiber cloth is ⁇ 500 ppm, more preferably 1000-8000 ppm.
- the fiber material used for fiber formation includes any one of natural fibers or fibers obtained by wet spinning. Specifically, it includes natural fibers such as cotton fibers, man-made cellulose fibers, and man-made fibers. At least one of protein fiber, polyacrylonitrile fiber, and polyvinyl alcohol fiber.
- the above-mentioned fibers all contain hydroxyl groups, and the fabrics obtained after forming the net on the netting curtain contain open hydroxyl groups, which can form chemical chelation with the complex copper ions when they are paddled in the organic complex copper solution.
- the combination is more tight, such as the fiber material is only viscose fiber or peanut protein fiber, or a mixture of viscose fiber and peanut protein fiber.
- the fabric obtained after the fiber material fiber web-forming step contains ⁇ 5wt% cotton fiber, or 5-65wt% cellulose fiber, or 5-65wt% protein fiber, or 5-65wt% polyacrylonitrile
- the fiber, or 100% low-temperature water-soluble polyvinyl alcohol fiber can use any one of the above-mentioned solutions, but is not limited to the above-mentioned solution.
- the fiber material is a mixed fiber material of the above-mentioned hydroxyl-containing fibers and non-hydroxyl-containing fibers, the sum of the hydroxyl-containing fibers in the fabric after the fiber is formed into the web can reach the corresponding minimum content, such as cotton fiber and viscose fiber.
- the low-temperature water-soluble polyvinyl alcohol fiber can be directly dissolved in low-temperature water, and can be dissolved in water at 20-98°C.
- the fiber material used for fiber formation such as the fiber material contains one or more of polyester fiber, polyamide fiber, polyvinyl chloride fiber, and polypropylene fiber, in order to improve the complex copper
- the chitosan-ascorbic acid solution padding step is also carried out before padding and sizing. Both chitosan and ascorbic acid contain open hydroxyl groups, and then the chitosan is used.
- the adsorption performance and the addition of acetic acid in the chitosan-ascorbic acid solution make the chitosan and ascorbic acid more firmly adhere to the spunlace fiber cloth base cloth, and complex copper ions in the organic complex copper solution to form chemical chelation to enhance the organic Bond strength between copper and spunlace fiber cloth.
- Preparation examples 1-5 are preparation examples of the organic complex copper solution.
- a preparation method of organic complex copper solution including the following steps:
- a preparation method of organic complex copper solution including the following steps:
- a preparation method of organic complex copper solution including the following steps:
- a preparation method of the organic complex copper solution is carried out according to the method in Preparation Example 2, except that the initial organic complex copper solution is poured into 15 volume multiples of pure water to prepare the organic complex copper solution.
- a preparation method of the organic complex copper solution is carried out according to the method in Preparation Example 2, except that the initial organic complex copper solution is poured into 25 volume multiples of pure water to prepare the organic complex copper solution.
- Preparation examples 6-10 are preparation examples of chitosan-ascorbic acid solution.
- a preparation method of chitosan-ascorbic acid solution includes the following steps:
- a preparation method of chitosan-ascorbic acid solution includes the following steps:
- a preparation method of chitosan-ascorbic acid solution includes the following steps:
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
- spunlace non-woven fabric base fabric the mixed fiber material of viscose fiber and polyester fiber is sequentially subjected to fiber web formation, pre-wetting, and spunlace reinforcement to obtain a spunlace fiber fabric base fabric.
- the fabric after fiber formation contains 5wt. % Of viscose fiber;
- the spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution by a sizing machine to obtain a copper-containing spunlace non-woven fabric.
- the organic complex copper solution in the sizing machine is prepared in Preparation Example 2 The organic complex copper solution;
- the copper-containing spunlace non-woven fabric obtained after padding and sizing is dried and wound at a drying temperature of 90°C.
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
- Spunlace non-woven fabric base fabric preparation the viscose fiber, polyacrylonitrile fiber and polyester fiber mixed fiber are sequentially fabricated, pre-wet, and spunlaced to obtain a spunlace fiber fabric base fabric.
- the sum of viscose fiber and polyester fiber in the cloth is 65wt%;
- the spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution by a sizing machine to obtain a copper-containing spunlace non-woven fabric.
- the organic complex copper solution in the sizing machine is prepared in Preparation Example 1 The organic complex copper solution;
- the copper-containing spunlace nonwoven fabric obtained after padding and sizing is dried and wound at a drying temperature of 100°C.
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
- Spunlace non-woven fabric base fabric preparation Spunlace fiber fabric base fabric is obtained by combining cotton fiber and polyester fiber mixed fiber through fiber web formation, pre-wetting, and spunlace reinforcement.
- the cotton fiber content in the fabric after fiber web formation is 5wt%;
- the spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution through a sizing machine to obtain a copper-containing spunlace non-woven fabric.
- the organic complex copper solution in the sizing machine is prepared in Preparation Example 5 The organic complex copper solution;
- the copper-containing spunlace nonwoven fabric obtained after padding and sizing is dried and wound at a drying temperature of 100°C.
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics is carried out according to the method in Example 2, except that:
- the soybean fiber and polyester fiber mixed fiber are sequentially subjected to fiber formation, pre-wetting, and spunlace reinforcement to obtain the spunlace fiber fabric base fabric.
- the content of soybean fiber in the fabric after the fiber formation is 20wt%;
- the organic complex copper solution in the sizing machine is the organic complex copper solution prepared in Preparation Example 3.
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics is carried out according to the method in Example 2, except that:
- the low-temperature water-soluble polyvinyl alcohol fiber is successively subjected to fiber web formation, pre-wetting, and spunlace reinforcement to obtain the spunlace fiber fabric base fabric.
- the low-temperature water-soluble polyvinyl alcohol can be Dissolve in the water temperature
- the organic complex copper solution in the sizing machine is selected from the organic complex copper solution prepared in Preparation Example 4.
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
- Spunlace fiber fabric base fabric is obtained after the polypropylene fiber is formed into a web, pre-wet, and spunlace reinforced in sequence;
- Chitosan-ascorbic acid solution padding In the sizing machine, the spunlace fiber cloth is padding in the chitosan-ascorbic acid solution, and then dried at 150°C for 10 minutes. The chitosan-ascorbic acid solution in the sizing machine is selected The chitosan-ascorbic acid solution prepared in Preparation Example 6;
- the dried spunlace fiber cloth base cloth is soaped in 5g/L soaping agent for 10 minutes, the soaping temperature is 35°C, and then dried at 50°C.
- the soaping agent is purchased from Dongguan Spinning Chain New Material Technology Co., Ltd., the brand is Texchain, the model is 605;
- the soaped spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution through the sizing machine to obtain the copper-containing spunlace non-woven fabric.
- the preparation example of the organic complex copper solution in the sizing machine The organic complex copper solution prepared in 1;
- the copper-containing spunlace nonwoven fabric obtained after padding and sizing is dried and wound at a drying temperature of 100°C.
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
- the polyamide fiber is successively subjected to fiber formation, pre-wetting, and spunlace reinforcement to obtain the spunlace fiber fabric base fabric;
- Chitosan-ascorbic acid solution padding In the sizing machine, the spunlace fiber cloth is padding in the chitosan-ascorbic acid solution, and then dried at 160°C for 8 minutes. The chitosan-ascorbic acid solution in the sizing machine is selected The chitosan-ascorbic acid solution prepared in Preparation Example 7;
- the dried spunlace fiber cloth base fabric is soaped in 5g/L soaping agent for 5 minutes, the soaping temperature is 40°C, and then dried at 55°C.
- the soaping agent is purchased from Dongguan Spinning Chain New Material Technology Co., Ltd., the brand is Texchain, the model is 605;
- the soaped spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution through the sizing machine to obtain the copper-containing spunlace non-woven fabric.
- the preparation example of the organic complex copper solution in the sizing machine The organic complex copper solution prepared in 2;
- the copper-containing spunlace nonwoven fabric obtained after padding and sizing is dried and wound at a drying temperature of 100°C.
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics includes the following steps:
- the polyvinyl chloride fiber is successively subjected to fiber web formation, pre-wetting, and spunlace reinforcement to obtain the spunlace fiber fabric base fabric;
- Chitosan-ascorbic acid solution padding In the sizing machine, the spunlace fiber cloth base cloth is padding in the chitosan-ascorbic acid solution, and then dried at 170°C for 5 minutes. The chitosan-ascorbic acid solution in the sizing machine is selected The chitosan-ascorbic acid solution prepared in Preparation Example 8;
- the dried spunlace fiber cloth base cloth is soaped in 5g/L soaping agent for 5 minutes, the soaping temperature is 40 °C, and then dried at 60 °C, of which, the soaping agent is purchased from Dongguan Spinning Chain New Material Technology Co., Ltd., the brand is Texchain, the model is 605;
- the soaped spunlace fiber cloth base fabric is padding sizing in the organic complex copper solution through the sizing machine to obtain the copper-containing spunlace non-woven fabric.
- the preparation example of the organic complex copper solution in the sizing machine The organic complex copper solution prepared in 3;
- the copper-containing spunlace nonwoven fabric obtained after padding and sizing is dried and wound at a drying temperature of 100°C.
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics is carried out according to the method in Example 2. The difference is that in the padding sizing step, when the organic complex copper solution in the sizing machine is prepared, the initial organic The copper complex solution was poured into pure water of 12 volume multiples, and the rest was the same as in Preparation Example 2.
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics is carried out according to the method in Example 2. The difference is that in the padding sizing step, when the organic complex copper solution in the sizing machine is prepared, the initial organic The copper complex solution was poured into pure water of 25 volume multiples, and the rest was the same as in Preparation Example 2.
- a method for preparing copper-containing antibacterial and antiviral non-woven fabrics is carried out according to the method in Example 2. The difference is that in the padding sizing step, the solution in the sizing machine is not an organic complex copper solution, but 3mol/ L of copper chloride solution.
- test sample is a disc with a diameter of 4.8 cm. 4 parallel tests are performed, and the average value is taken.
- the tested strain is Methicillin-resistant Staphylococcus aureus ATCC 33591, the inoculation volume is 1 mL, and the test results are shown in Table 1 below.
- the antibacterial properties of the spunlace nonwoven fabric prepared by the method of this application are good, especially for methicillin-resistant Staphylococcus aureus, which is more toxic and drug resistant, and its antibacterial properties are still relatively good.
- the copper ion concentration in the initial organic complexed copper solution in this application is 5.5wt%, adding 10-30 volume multiples of water, combined with the control of the fiber material used for fiber web formation, can control the spunlace nonwoven
- the amount of copper ions on the cloth is between 500ppm-8000ppm, which has a good antibacterial effect.
- the spunlace non-woven fiber material in Examples 1-5 is a fiber containing hydroxyl groups.
- the raw material of the spunlace non-woven fabric is synthetic polyester.
- the fiber does not contain cellulose. It is first dipped in a chitosan-ascorbic acid solution and then dipped in an organic complex copper solution.
- the final spunlace non-woven fabric also has good antibacterial properties.
- Example 2 The spunlace non-woven fabrics obtained in Example 2, Example 7 and Comparative Examples 1 and 3 were washed 50 times, 100 times and 200 times, respectively, and then referenced to AATCC 100-2012 textile antibacterial performance test.
- the test sample is the diameter It is a 4.8 cm disc, the tested strain is methicillin-resistant Staphylococcus aureus ATCC 33591, and the volume of the inoculation is 1 mL.
- the copper content on the spunlace non-woven fabric is tested to determine the copper content loss, and the test The results are shown in Table 3 below.
- the spunlace non-woven fabric prepared in Example 2 was tested for influenza A virus H1N1 according to the standard of ISO 18184:2014(E) "Anti-Virus Textile Testing".
- the experimental group and the control group were set up, and the virus strain was prevented by China Influenza A virus A/PR8/34 (H1N1) provided by the Institute of Virology, Academy of Medical Sciences, the cell line is a continuous canine kidney epithelial cell line MDCK cells, purchased from ATCC, the logarithm value of the virus titer of the test group samples after inoculation and incubation for 24 hours (lgTCID 50 /bottle) The average value is 3.48, the antiviral activity value is 3.08, the antiviral activity rate is 99.92%, and the antiviral activity is good.
- the copper-containing spunlace non-woven fabric prepared in this application was tested and evaluated for anti-virus, and mouse Noro s99 was used instead of human Norovirus to perform the inactivation residual activity test on human skin. It is verified that the copper-containing non-woven fabric can inactivate the virus on the human skin within 4 hours.
- the experimental group and the control group are set up and 5 parallel tests are carried out.
- the skin is provided by the human subcutaneous tissue of the British Tissue Solutions Limited company.
- the virus is selected in Murine norovirus s99 Berlin strain/RAW cells stored at -80°C and isolated from mouse RAW cells, the virus number is MNV 260315.17, the test steps are as follows:
- Example 2 Use the wet copper-containing spunlace nonwoven fabric prepared in Example 2 to perform standard wiping action on the surface of the subcutaneous tissue sample (1.0 ⁇ 1.0cm): fix the subcutaneous tissue sample with sterile tweezers, and then use the copper-containing spunlace The non-woven fabric wipes 3 times along the surface of the subcutaneous tissue sample, and wipes 3 times at 90°C, and then repeats this process for a duration of 30s.
- the above-mentioned wiping process is carried out in a separate sterile plastic petri dish;
- DMEM medium is Dulbecco's modified Eagle medium
- a sample of the filtrate in a volume of 0.1ml was passed through gel filtration (Microspin S-400 HR chromatographic column), and the eluent was serially diluted 10 times for TCID 50 analysis.
- TCID 50 was calculated for all 5 groups of parallel experiments.
- TCID 50 is calculated according to the Karber method.
- the virus in the eluate is calculated as 10 ( ⁇ n+0.5) ⁇ 400 TCID50/ml, where ⁇ n is the sum of the proportions of infected wells from 10 -1 to 10 -6 virus dilution.
- the murine norovirus s99 Berlin strain/RAW cell was used as a substitute for human norovirus to perform a virus test on human skin.
- the logarithmic value of the virus titer of the experimental group in Example 2 of this application (lgTCID 50 /bottle) The average value is 4.00, and the antiviral activity is good.
- the biological activity of the virus on the human skin in the experimental group was reduced by 57.32% on average after the copper-containing spunlace non-woven fabric treatment, verifying that the human skin was wiped with the copper-containing spunlace non-woven fabric for 4 hours to inactivate the virus The effect verifies the excellent antiviral performance of the copper-containing spunlace non-woven fabric.
- the spunlace non-woven fabric obtained by the method provided in this application has antibacterial and anti-viral properties, and can be widely used in medical and sanitary non-woven fabrics, non-woven fabrics for home decoration, non-woven fabrics for clothing, and non-woven fabrics for industrial use.
- Fabrics, agricultural non-woven fabrics and other fields, especially using its antibacterial and antiviral properties in medical and health products such as masks, surgical gowns, etc. have a wide range of applications.
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Abstract
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US20220061327A1 (en) * | 2020-08-28 | 2022-03-03 | Uop Llc | Antiviral metal treatments for fiber substrates, filter media having antiviral metal treatments, and processes for treating fiber substrates |
CN114395913A (zh) * | 2022-01-13 | 2022-04-26 | 南通恒绮纺织有限公司 | 一种舒适耐用的棉纺织物及制作工艺 |
CN115478331A (zh) * | 2022-09-29 | 2022-12-16 | 博升(武汉)服装有限公司 | 一种缓释杀菌消光剂及其制备方法和高弹力文胸 |
CN115652614A (zh) * | 2022-10-26 | 2023-01-31 | 福建龙美医疗器械有限公司 | 一种医用抗菌抗病毒水刺无纺布及制备方法 |
CN115652625B (zh) * | 2022-11-15 | 2024-03-12 | 中南大学湘雅三医院 | 一种带有纳米铜和紫草素的无纺布及其制备方法 |
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