Antibacterial and antiviral fabrics, softcoat formulations, and methods of making the same
The nano-adhesive particle coating with a three-dimensional porous network structure solves the problem of incompatibility between soft surface antibacterial coatings and substrates, achieving high-efficiency antibacterial effect and breathability, and is suitable for personal protective equipment.
Patent Information
- Application Number
- CN202310365075.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Priority Date
- 2023-04-06
- Filing Date
- 2023-04-07
- Publication Date
- 2025-11-11
- Estimated Expiration
- 2043-04-07
Smart Images

Figure CN116892125B_ABST
Abstract
Description
[0001] Cross-references to related applications
[0002] This application claims priority to U.S. Patent Application No. 63 / 329,493, filed April 11, 2022, and U.S. Patent Application No. 18 / 296,962, filed April 6, 2023, the disclosures of which are incorporated herein by reference. Technical Field
[0003] This invention generally relates to a nano-adhesive particle coating. More specifically, this invention relates to antibacterial and antiviral fabrics for soft surfaces and antibacterial and antiviral formulations, and also to antibacterial and antiviral nanoparticles and methods for their preparation. Background Technology
[0004] Antimicrobial coatings contain an antimicrobial agent that kills, inhibits, or reduces bacterial growth on the coating surface. However, the performance of conventional antimicrobial coatings is highly dependent on their bonding system and the coating substrate. Incompatibility between the coating and the substrate can affect antimicrobial performance. For example, rigid antimicrobial coating films are unsuitable for soft surfaces because their mechanical properties are inconsistent with those of soft substrates, and coatings with conventional bonding systems (intact layers) obstruct the porous structure of the substrate and restrict mechanical movement. Therefore, there is a need for an antimicrobial coating for soft surfaces that provides a high surface area for sustainably released antimicrobial agents, has high porosity to absorb mechanical energy, and high interparticle connectivity to provide flexible adhesion on soft surfaces.
[0005] Previous antimicrobial hard coatings were described in "Durable Antimicrobial Coating Compositions" (US9957396B2, CN105295558B and HK1213937A1) and "Durable, Bactericide-Free Antimicrobial Coatings" (US20140242363A1 and HK1196633A1). This antimicrobial hard coating exhibits antimicrobial properties against Gram-positive bacteria (Staphylococcus aureus), Gram-negative bacteria (Escherichia coli), methicillin-resistant Staphylococcus aureus (MRSA), and extended-spectrum β-lactamase (ESBL)-resistant Klebsiella pneumoniae, demonstrating a 99.9% removal rate within 15 minutes. Third-party laboratory certification confirms its antiviral (removal of 99.9% of H1N1 within 10 minutes, test standard according to JIS Z 2801), endospore-killing (removal of 99.9% of Bacillus subtilis within 60 minutes, test standard according to JIS Z28001), and antifungal (no growth within 6 weeks, test standard according to BS3900-G6:1989) effects. The coating has been shown to maintain its antimicrobial effect for up to 9 months.
[0006] US Patent 9616021B2 discloses zein-based nanoparticles formed by freeze-drying to reduce immunogenicity induced by large-sized particles. The particle size ranges from 100 nm to 400 nm. The pH of the reaction solution is approximately 6.8 to 7.4. The concentration of the active ingredient, zein particles, in the solution is approximately 10 mg / mL. After freeze-drying, the encapsulation efficiency of the zein particles is approximately 60% to 80%.
[0007] US Patent 20080147019A1 discloses an antimicrobial composition comprising a chitosan-based matrix having 0.01% to 15% by weight of metal nanoparticles with a size of 1 nanometer to 250 nanometers. The total weight percentage of chitosan or chitosan derivative compounds in the matrix is at least 10%, the total weight percentage of a crosslinking agent in the matrix is 0% to 10%, and the total weight percentage of a chemical or physical modifier in the matrix is up to about 60%. This chemical agent possesses antimicrobial properties, capable of killing microorganisms or inhibiting their growth on a solid matrix.
[0008] International patent application WO2016156939A1 discloses a composite material containing chitosan and zinc oxide nanoparticle aggregates for sun protection. The zinc oxide particles are trapped in chitosan crosslinked with tripolyphosphate ions. The viscosity of the chitosan solution ranges from 200 cP to 800 cP, and the zinc oxide particle size is no greater than 100 nanometers. The aggregate size is no greater than 100 micrometers.
[0009] US Patent 8349343B2 discloses an antibacterial treatment of textile materials using polymer / chitosan core-shell particles dispersed in water. The polymer / chitosan core-shell particles are formulated from 0.1% to 10% of an acidic solution containing vinyl monomers, chitosan, and a hydrogen peroxide initiator at a weight ratio of 0.5-50:1 (w / w). The resulting polymer particle suspension is coated onto the fabric by immersion. The coated fabric is then padded and dried in an oven at 100°C for 5 minutes. This process is repeated several times, and finally, the fabric is cured in an oven at 150°C for 4 minutes to form the final coating.
[0010] However, the particles / coatings from the aforementioned prior art involve complex synthesis processes, and the resulting particles / coatings are unsuitable for soft surface applications. Furthermore, existing technologies fail to provide coatings with high porosity and nanostructures. Intact and rigid solid films can clog the porous structure of fabrics, further affecting the breathability and filtration performance of the coated surface. Moreover, these conventional coatings are prone to peeling off after a period of use, eventually losing their function because they are inelastic and incompatible with soft surfaces.
[0011] Therefore, there is a need to develop an antimicrobial coating for soft substrates. This invention addresses this need. Summary of the Invention
[0012] In a first aspect, the present invention provides an antimicrobial and antiviral (ABV) fabric comprising a fabric substrate and an antimicrobial coating formed on the fabric substrate. The coating formed on the fabric substrate has an antimicrobial agent embedded or surface-adhered in a three-dimensional porous network of nano-adhesive particles.
[0013] In one embodiment, the antimicrobial agent comprises at least two antimicrobial components selected from polyhexamethylene biguanide, chlorhexidine, zinc pyrithione, gallic acid, nisin, and silane quaternary ammonium compounds. Antimicrobial coatings containing at least two antimicrobial components exhibit a synergistic effect, providing both rapid action and durability.
[0014] In one embodiment, the nano-adhesive particles comprise at least two adhesive components selected from chitosan, zein, gelatin, cellulose, alginate, pectin, acrylic latex, polyurethane, cyclodextrin, silica, zinc oxide, titanium dioxide, copper oxide, and iron oxide.
[0015] In one embodiment, at least two antimicrobial components are embedded or surface-adhered to a three-dimensional nano-adhesive system. The three-dimensional network coating on the soft surface is formed by interconnecting nanoparticles through van der Waals or Coulomb forces, and these particles contribute to the formation of unique structures due to their size and surface properties.
[0016] Compared to traditional adhesives, the voids and channels in the three-dimensional porous network allow air and moisture to permeate into the fabric. Furthermore, the three-dimensional porous network of nano-adhesive particles absorbs compressive and tensile forces by deforming the three-dimensional porous network, thereby increasing the membrane's mechanical resilience. In addition, the porous structure increases the exposure of antimicrobial components by providing a high surface area.
[0017] In one embodiment, the fabric substrate is selected from polypropylene (PP) substrates, polyethylene (PE) substrates, polyester substrates, cotton substrates, nylon, spandex substrates, cotton-polyester blends, cotton-nylon blends, and cotton-spandex blends. The antimicrobial coating can be applied to the soft substrate by spraying, dipping, scraping, backing dry curing, or wiping. It should be understood that curing this coating on a soft substrate does not require heat treatment.
[0018] In another embodiment, the three-dimensional porous network has pores surrounded by nano-binder particles, and the average pore size of the three-dimensional porous network is at least 50 nanometers.
[0019] In yet another embodiment, an antimicrobial agent is embedded in or adhered to the surface of nano-adhesive particles to form antibacterial and antiviral nanoparticles with a particle size of 100 nanometers to 800 nanometers.
[0020] In another embodiment, the antibacterial and antiviral nanoparticles have a polydispersity of 0.05 to 0.5.
[0021] In one embodiment, the antimicrobial and antiviral fabric is breathable, with an increased surface area of at least about 1000% and an increased porosity of at least about 1000% compared to an uncoated fabric.
[0022] In one embodiment, the antimicrobial and antiviral fabric has an antimicrobial effect of at least 99% while retaining physical properties comparable to uncoated fabric.
[0023] In a second aspect, the invention also relates to two antibacterial and antiviral coating formulations, one of which is a formulation for direct spraying onto soft surfaces such as polymers, nonwovens, and fabrics. The other formulation is for addition to polymer inks used in soft-surface applications.
[0024] In one embodiment, the present invention provides an antimicrobial and antiviral formulation for soft surfaces, comprising 0.01% to 5% by weight of an antimicrobial agent, 0.01% to 5% by weight of nano-binder particles, and a surfactant and a solvent.
[0025] In another embodiment, the antimicrobial agent has at least two antimicrobial components selected from polyhexamethylene biguanide, chlorhexidine, zinc pyrithione, gallic acid, nisin, and silane quaternary ammonium compounds. The nano-binder particles have at least two binder components selected from chitosan, zein, gelatin, cellulose, alginate, pectin, acrylic latex, polyurethane, cyclodextrin, silica, zinc oxide, titanium dioxide, copper oxide, and iron oxide.
[0026] In yet another embodiment, the formulation further includes a crosslinking agent selected from the group consisting of tripolyphosphate (TPP), glutaraldehyde, critical acid, adipic acid, 1,2,3,4-butanedicarboxylic acid (BTCA), methoxy polyethylene glycol aldehyde, and dimethyloldihydroxyethylene urea, in an amount of 0.01% to 1% by weight.
[0027] In another embodiment, the solvent comprises a first solution and a second solution. The first solution is selected from water, ethyl acetate, isopropanol, ethanol, acetic acid, ammonia, or combinations thereof, and the second solution is selected from isopropyl myristate (IPM), isopropyl palmitate, oleic acid, almond oil, soybean oil, or combinations thereof. The surfactant is selected from cetrimonium bromide (CTAB), polysorbate 20, polysorbate 80, sorbitol laurate, sorbitol oleate, polyglycerol-6-caprylate, polyglycerol-3-cocoate, polyglycerol-4-decanoate, polyglycerol-6-ricinoleate, or combinations thereof.
[0028] In one embodiment, the surfactant is used in an amount of 0.01% to 10% by weight, and the solvent is used in an amount of 85.0% to 99.5% by weight. Specifically, the surfactant is used in an amount of 0.01% to 10% by weight, the first solution is used in an amount of 85.0% to 99.5% by weight, and the second solution is used in an amount of 0.01% to 5% by weight.
[0029] In a third aspect, the present invention also provides a method for preparing antibacterial and antiviral nanoparticles, comprising: step (a) providing a first mixture comprising at least one antimicrobial component and at least one binder component;
[0030] Step (b) homogenizes the first mixture; and
[0031] Step (c) involves adding at least one other antimicrobial component and at least one other binder component, and mixing them with the first mixture to form a second mixture, wherein antibacterial and antiviral nanoparticles are formed in the second mixture.
[0032] Antimicrobial components are embedded in or adhered to the surface of nano-adhesive particles to form antibacterial and antiviral nanoparticles.
[0033] In one embodiment, the antimicrobial component and the adhesive component are present in a weight percentage of 0.01% to 5% based on the weight of the second mixture.
[0034] In one implementation, the pressure in step (b) is in the range of 0 bar to 1000 bar.
[0035] In another implementation, the pressure in step (b) is in the range of 200 bar to 700 bar.
[0036] In one embodiment, step (a) or step (c) further includes the addition of a surfactant in an amount of about 0.01 to 10% by weight and a solvent in an amount of about 85.0% to 99.5% by weight.
[0037] In one embodiment, step (b) further includes a heat treatment step at 40°C to 70°C.
[0038] In one embodiment, the antimicrobial component includes polyhexamethylene biguanide, chlorhexidine, zinc pyrithione, gallic acid, nisin, or a silane quaternary ammonium compound, and the adhesive component includes chitosan, zein, gelatin, cellulose, alginate, pectin, acrylic latex, polyurethane, cyclodextrin, silica, zinc oxide, titanium dioxide, copper oxide, or iron oxide.
[0039] The present invention has the following advantages:
[0040] (1) This invention provides a coating with effective antimicrobial function, high durability and stability. The preparation of this coating is simple and it can be cured or dried without heat treatment.
[0041] (2) The difference in particle filtration efficiency, air permeability and moisture permeability between coated and uncoated fabrics is less than 10%, which means that coated fabrics retain similar physical properties to uncoated fabrics. In other words, nano-adhesive particles do not completely block the surface of the substrate.
[0042] (3) The coating substrate has good air permeability and moisture permeability, which is beneficial for application in personal protective equipment (such as masks or disposable gowns).
[0043] (4) The resulting coating has better compatibility with soft substrates and high antibacterial effect. Even after several washes, the coated substrate still maintains high antibacterial effect. Attached Figure Description
[0044] In the following detailed description, exemplary, non-limiting, and non-exhaustive embodiments of the invention are described with reference to the accompanying drawings. For a more detailed understanding of the features of the invention described above, a more detailed description of the invention can be obtained by referring to the accompanying drawings of some embodiments, which are briefly summarized above. However, it should be noted that these drawings only illustrate typical embodiments of the invention and should not be considered as limiting its scope; other equally effective embodiments are permissible with respect to the invention.
[0045] Figure 1 This illustrates a comparison between conventional adhesives coated on soft surfaces and nano-adhesive particles coated on soft surfaces.
[0046] Figure 2 The process for fabricating the antibacterial and antiviral nanoparticles in Examples 1-4 is explained.
[0047] Figure 3 The process for fabricating the antibacterial and antiviral nanoparticles in Examples 2-3 is explained.
[0048] Figure 4A The particle size distribution of the antibacterial and antiviral nanoparticles of Examples 1-4 is depicted.
[0049] Figure 4B The particle size distribution of the antibacterial and antiviral nanoparticles of Examples 2-3 is depicted.
[0050] Figure 5 The images show photographs of the coated PP substrate, uncoated PP substrate, coated PE substrate, and uncoated PE substrate of Example 3.
[0051] Figure 6 The images show the antibacterial and antiviral formulations of Examples 1-4, the coated mask of Example 4, and the coated disposable gown.
[0052] Figure 7 SEM images showing a PP substrate coated with antibacterial and antiviral nanoparticles ((a) 5000x magnification (b) 20000x magnification) and a PE substrate coated with antibacterial and antiviral nanoparticles ((c) 5000x magnification (d) 20000x magnification).
[0053] Figure 8 The image shows (a) the PALAs MFP 1000HPA filter testing system, (b) the location of the sample, (c) the user interface, and (d) photos of the test parameters.
[0054] Figure 9 The image shows (a) the FX 3360 portable air permeability tester and (b) the test parameters.
[0055] Figure 10 The image shows (a) the TF165B fully automatic water vapor permeability tester, (b) the permeation cup with the sample, and (c) the calculation method and test parameters.
[0056] Figure 11 Explain the screen printing process.
[0057] Figure 12 Explain the heat transfer printing process.
[0058] Figure 13 The images show (a) the first antibacterial and antiviral ink of Example 7, (b) a polyester substrate printed with the first antibacterial and antiviral ink, (c) the second antibacterial and antiviral ink of Example 7, and (d) a polyester substrate hot-melt printed with the second antibacterial and antiviral ink.
[0059] Figure 14A This is a picture of a fabric touch tester.
[0060] Figures 14B to 14F It is a graph of the measured parameters.
[0061] Figure 15 These are images of the inhibition zones of the antibacterial and antiviral formulations in Examples 1-4.
[0062] Figure 16 These are images of the inhibition zone test results for the antibacterial and antiviral formulations of Examples 2-3.
[0063] Figure 17 These are test images of the inhibition zone of a PP substrate coated with an antibacterial and antiviral formula.
[0064] Figure 18 These are test images of the inhibition zone of a polyester substrate coated with an antibacterial and antiviral formula. Detailed Implementation
[0065] Rigid antibacterial coatings are unsuitable for soft surfaces because their mechanical properties are inconsistent with those of the soft substrate, and coating with conventional bonding systems can clog the substrate's pore structure. Therefore, this invention provides an antibacterial and antiviral fabric, a formulation for a soft coating, and a method for preparing antibacterial and antiviral nanoparticles.
[0066] First, the antimicrobial and antiviral fabric comprises a fabric substrate and an antimicrobial coating. In particular, the fabric is a flexible substrate. It should be understood that the term "flexible substrate" in this specification refers to a flexible, bendable, and deformable substrate.
[0067] Specifically, the fabric substrate is expected to include, but is not limited to, polypropylene substrate, polyethylene substrate, polyester substrate, cotton substrate, nylon substrate, spandex substrate, cotton-polyester blend, cotton-nylon blend, or cotton-spandex blend. In one embodiment, the coated fabric is selected for medical use.
[0068] The antimicrobial coating formed on the fabric substrate has an antimicrobial agent embedded or surface-adhered in a three-dimensional porous network of nano-adhesive particles, as shown in the schematic diagram of the three-dimensional porous network. Figure 1 As shown.
[0069] Antimicrobial agents include at least two antimicrobial components, which are expected to include, but are not limited to, polyhexamethylene biguanide, chlorhexidine, zinc pyrithione, gallic acid, nisin, and silane quaternary ammonium compounds.
[0070] The nano-binder particles comprise at least two binder components, which are expected to include, but are not limited to, chitosan, zein, gelatin, cellulose, alginate, pectin, acrylic latex, polyurethane, cyclodextrin, silica, zinc oxide, titanium dioxide, copper oxide, and iron oxide.
[0071] In one embodiment, the particle filtration efficiency of the coated fabric is higher than that of the uncoated fabric. Preferably, the particle filtration efficiency of the coated fabric is improved by at least 5% compared to the uncoated fabric, and it is suitable for hygiene products.
[0072] Preferably, the three-dimensional network has pores surrounded by nano-binder particles, and the three-dimensional network has an average pore size of at least 50 nanometers. The pores and voids formed in the coating allow gas and moisture to permeate. Adjacent nano-binder particles are interconnected by van der Waals forces or Coulomb forces. Depending on the characteristics of the antimicrobial and binder components, the pore size can be between 20 nanometers and 500 nanometers, or between 30 nanometers and 100 nanometers. A suitable pore size is important for breathable materials, especially face masks.
[0073] Antimicrobial agents are embedded in or adhered to the surface of nano-adhesive particles to form antibacterial and antiviral nanoparticles with a particle size between 100 nanometers and 800 nanometers, or between 100 nanometers and 600 nanometers.
[0074] The polydispersity of the nanoparticles ranges from 0.05 to 0.5 or from 0.05 to 0.2.
[0075] The coated substrate exhibits at least 99% antimicrobial efficacy against *Escherichia coli*, *Staphylococcus aureus*, human coronavirus, *Bacillus subtilis*, *Aspergillus brasiliensis*, *Pseudomonas cordifolia*, *Candida albicans*, *Trichoderma viride*, and *Aureobasidium aeruginosa*. Furthermore, the coated substrate is washable and exhibits high wash resistance. The coated substrate retains its high antimicrobial efficacy after washing. Preferably, the coated substrate exhibits 99.5% or higher antimicrobial efficacy after washing.
[0076] In one embodiment, the coated and uncoated substrates have similar mechanical properties, such as stiffness and surface parameters (e.g., surface roughness).
[0077] The coated substrate meets chemical and biological safety requirements and is suitable for personal protective equipment (PPE).
[0078] In one embodiment, the coated substrate has a density of 0.05 g / cm³. 2 Up to 0.06 g / cm 2 The weight of the coating.
[0079] Secondly, this invention also provides an antimicrobial and antiviral formulation for soft surfaces. The antimicrobial and antiviral formulation includes an antimicrobial agent, nano-adhesive particles, a surfactant, and a solvent. The antimicrobial agent can be embedded or surface-adhered in a three-dimensional network of nano-adhesive particles, or simply dispersed in the formulation. The antimicrobial and antiviral nanoparticles are essentially nano-adhesive particles with embedded or surface-adhered antimicrobial agents, and the particle size is in the range of 100 nanometers to 800 nanometers. The antimicrobial and antiviral formulation can be applied to soft substrates such as polypropylene matrices, polyethylene matrices, and polyester matrices.
[0080] In particular, the antimicrobial and antiviral formulations include 0.01% to 5% by weight of an antimicrobial agent, 0.01% to 5% by weight of nano-binder particles, surfactants, and solvents. The antimicrobial agent has at least two antimicrobial components, which are expected to include, but are not limited to, polyhexamethylene biguanide, chlorhexidine, zinc pyrithione, gallic acid, nisin, and silane quaternary ammonium compounds. The nano-binder particles have at least two binder components, which are expected to include, but are not limited to, chitosan, zein, gelatin, cellulose, alginate, pectin, acrylic latex, polyurethane, cyclodextrin, silica, zinc oxide, titanium dioxide, copper oxide, and iron oxide.
[0081] Preferably, the antimicrobial agent comprises two antimicrobial components. This combination of antimicrobial components can be a mixture of chlorhexidine and PHMB, or a mixture of chlorhexidine and zinc pyrithione. These combinations have a high affinity for nano-binder particles, thereby producing a greater antimicrobial effect.
[0082] Preferably, the nano-adhesive particles are a mixture of zein, chitosan, and zinc oxide, or a mixture of zein and chitosan. When these nano-adhesive particles are coated on a soft surface, they can absorb compressive and tensile forces by deforming the three-dimensional network, thereby increasing the surface's mechanical resistance. Furthermore, the high surface area of the nano-adhesive particles facilitates the exposure of antimicrobial agents, resulting in a more significant antimicrobial effect.
[0083] Preferably, the surfactant is 0.01% to 10%, 0.01% to 5%, or 0.01% to 2% by weight, and the solvent is 85% to 99.5%, 90% to 99.5%, or 92% to 99.5% by weight.
[0084] Specifically, the solvent includes a first solution and a second solution. The first solution is expected to include, but is not limited to, water, ethyl acetate, isopropanol, ethanol, acetic acid, ammonia, or combinations thereof. The second solution is expected to include, but is not limited to, isopropyl myristate, isopropyl palmitate, oleic acid, almond oil, soybean oil, or combinations thereof. Depending on the solvent and surfactant, a water-in-oil emulsion system or an oil-in-water emulsion system can be used. Preferably, the formulation is an oil-in-water system.
[0085] Preferably, the first solution is 85% to 99.5% by weight, 90% to 99.5% by weight, or 92% to 99.5% by weight, and the second solution is 0.01% to 5% by weight, 0.01% to 3% by weight, or 0.01% to 1% by weight.
[0086] Optionally, the formulation includes 0.01% to 1%, 0.01% to 0.5%, or 0.01% to 0.1% by weight of a crosslinking agent. The crosslinking agent is contemplated, but is not limited to, tripolyphosphate, glutaraldehyde, citric acid, adipic acid, 1,2,3,4-butanetetracarboxylic acid, methoxy polyethylene glycol aldehyde, or dimethyloldihydroxyethylidene urea. Preferably, the crosslinking agent is citric acid, adipic acid, genipin, or 1,2,3,4-butanetetracarboxylic acid (BTCA), which is a suitable crosslinking agent for formulations of personal protective equipment because such crosslinking agents are non-toxic materials.
[0087] Antibacterial and antiviral formulations are applied to a substrate by spraying, dipping, scraping, drying with a pad, or wiping. The substrate may be, but is not limited to, polypropylene, polyethylene, polyester, cotton, nylon, spandex, cotton-polyester blends, cotton-nylon blends, or cotton-spandex blends.
[0088] Third, the present invention also provides a method for preparing antibacterial and antiviral nanoparticles:
[0089] Step (1): Provide a first mixture having at least one antimicrobial component and at least one adhesive component.
[0090] Step (2): Homogenize the first mixture.
[0091] Step (3): Add at least one other antimicrobial ingredient and at least one other adhesive ingredient to form a second mixture.
[0092] The antimicrobial ingredients are expected to include, but are not limited to, polyhexamethylene biguanide, chlorhexidine, zinc pyrithione, gallic acid, nisin, and silane quaternary ammonium compounds, as well as binder ingredients such as chitosan, zein, gelatin, cellulose, alginate, pectin, acrylic latex, polyurethane, cyclodextrin, silica, zinc oxide, titanium dioxide, copper oxide, and iron oxide.
[0093] The antimicrobial component is present in a weight percentage of 0.01% to 5% based on the weight of the second mixture, and the adhesive component is present in a weight percentage of 0.01% to 5% based on the weight of the second mixture.
[0094] In one embodiment, the first mixture comprises at least two antimicrobial components and at least one adhesive component. In another embodiment, the first mixture comprises at least one antimicrobial component and at least two adhesive components. In yet another embodiment, the first mixture comprises at least two antimicrobial components and at least two adhesive components.
[0095] In step (2), the homogenization pressure is in the range of 0 bar to 1000 bar or 200 bar to 700 bar, the homogenization time is in the range of 20 minutes to 60 minutes or 20 minutes to 40 minutes, and the homogenization speed is in the range of 1000 rpm to 2000 rpm, depending on the particle size of the nanoparticles. The homogenization speed is optimized to maintain the desired particle size. Higher homogenization speeds can prevent nanoparticle aggregation. Typically, high-speed and high-pressure homogenization methods are used to produce emulsions, which are oil-water or oil-water phases in the same liquid phase; this method is rarely used to produce solid particles.
[0096] In step (2), heat treatment may optionally be included. In one embodiment, the heat treatment ranges from 40°C to 70°C or from 50°C to 60°C. The heat treatment promotes the formation of particles in the first mixture having nanoscale size and spherical shape.
[0097] Step (2) also includes an antisolvent precipitation process. Preferably, the solvent used in the antisolvent process is water. The antisolvent precipitation process reduces the particle size distribution (polydispersity), which makes the nanoparticles more suitable for soft surfaces because the uniform particle size contributes to controllable air permeability in the coated substrate.
[0098] Optionally, a surfactant is added in step (2) or step (3). The surfactant can reduce the surface tension of the first or second mixture, and the nanoparticles formed in the second mixture will have a controllable size and shape. Increasing the amount of surfactant can also reduce the particle size.
[0099] Example
[0100] The examples and embodiments described herein are for illustrative purposes only and will suggest various modifications or variations to be made thereto by those skilled in the art, and are contained within the spirit and scope of this application. Furthermore, any element or limitation of any invention or embodiment thereof disclosed herein may be combined with any and / or all other elements or limitations (alone or in any combination) or any other invention or embodiment thereof disclosed herein, and all such combinations are covered within, but not limited to, the scope of this invention.
[0101] Example 1
[0102] Example 1-1
[0103] Prepare a 1% (w / w) zein solution
[0104] To prepare a 1% (by weight) zein solution, 1 gram of zein was dissolved in 99 grams of 80% ethanol solution. The mixture was heated at 50°C and stirred at 400 rpm for at least 30 minutes. The mixture was then cooled to room temperature and filtered through a 0.45-micron nylon mesh filter to remove undissolved residues, yielding a 1% (by weight) zein solution.
[0105] Examples 1-2
[0106] Prepare a 0.1% (w / w) chitosan / 2% chlorhexidine solution.
[0107] Dissolve 0.1 g of low molecular weight (less than 100 kDa) chitosan in a 1% acetic acid solution and stir the mixture at 400 rpm for at least 30 minutes. Then add 2 g of chlorhexidine to the mixture and stir at 400 rpm for at least 30 minutes to obtain a 0.1% chitosan / 2% chlorhexidine solution by weight.
[0108] Examples 1-3
[0109] Prepare a 0.2% (w / w) polyhexamethylene biguanide (PHMB) solution.
[0110] Dissolve 0.2 g of PHMB and 0.05 g of citric acid in 99.75 g of deionized water, and then stir the mixture at 400 rpm for at least 30 minutes to obtain a PHMB solution with a weight percentage of 0.2%.
[0111] Examples 1-4
[0112] Preparation of antibacterial and antiviral formulations
[0113] 20 mL of a 1% (w / w) zein solution was added to 1 mL of a 0.1% (w / w) chitosan / 2% chlorhexidine solution. The mixture was heated at 50°C for 5 minutes and homogenized at high speed for 5 minutes to produce a nano-binder mixture. Then, 0.02 g of cetyltrimethylammonium bromide (CTAB) and 0.02 g of isopropyl myristate (IPM) were dissolved in the nano-binder mixture. The mixture was transferred to a high-pressure homogenizer at 300 bar for 30 minutes. The resulting homogenized solution was collected, and 19 mL of a 0.05% (w / w) aqueous citric acid solution was added to the homogenized solution, and the mixture was stirred at 600 rpm for at least 30 minutes. The nano-binder center particles were formed during the antisolvent precipitation process. 4 mL of a 0.2% (w / w) PHMB solution was added to modify the nano-binder center particles, thereby forming antibacterial and antiviral nanoparticles. The process is as follows: Figure 2 As shown. The antibacterial and antiviral formulations of Example 1 are listed in Table 1.
[0114] Example 2
[0115] Example 2-1
[0116] Preparation of ZnO nanoparticles
[0117] 3 g of zinc nitrate was dissolved in 100 mL of water containing 1 g of gum arabic as a stabilizer, and preheated in a 450 W microwave for 2 minutes. The pH of the mixture was then adjusted to 10 with 0.1 M sodium hydroxide solution. An amorphous ZnO precipitate was formed, turning the mixture milky white. The mixture was then microwaved for 5 minutes to form ZnO nanoparticles. The ZnO nanoparticles were separated by centrifugation (10,000 rpm, 30 minutes), and the solid was dried overnight at 50 °C.
[0118] Example 2-2
[0119] Prepare a 1% (w / w) zein solution and a 0.1% (w / w) chitosan / 2% chlorhexidine solution. solution
[0120] The preparation methods for the 1% zein solution and the 0.1% chitosan / 2% chlorhexidine solution by weight are the same as those in Example 1.
[0121] Example 2-3
[0122] Preparation of antibacterial and antiviral formulations
[0123] Weigh 0.1 g of ZnO nanoparticles, 0.1 g of zinc pyrithione, 0.05 g of CTAB, and 0.05 g of IPM, and add them to 100 mL of a 0.1% (w / w) chitosan / 2% chlorhexidine solution. Homogenize the mixture for 30 minutes using a high-pressure homogenizer at 300 bar. Add 2.5 mL of a 1% (w / w) zein solution to the mixture and stir for at least 30 minutes. Antibacterial and antiviral nanoparticles are formed during the anti-precipitation process of the zein solution. The antibacterial and antiviral formulations of Example 2 are listed in Table 1. The manufacturing process is as follows: Figure 3 As shown.
[0124] Table 1
[0125]
[0126]
[0127] The particle size and polydispersity of the antibacterial and antiviral nanoparticles of Examples 1-4 and Examples 2-3, as measured by Zetasizer, are listed in Table 2. The size distribution maps are shown in Table 2. Figure 4A and 4B middle.
[0128] Table 2
[0129]
[0130] Example 3
[0131] Preparation of antibacterial and antiviral substrates
[0132] Polypropylene (PP) and polyethylene (PE) substrates are mounted on cardboard. 20 ml of the antibacterial and antiviral formulations from Examples 1-4 are filled into the spray gun's reservoir. The spray distance is set to 15 cm from the surface of the PP or PE substrate. The solution is sprayed horizontally from left to right, then from top to bottom, as a single coating. Three coats are applied to each substrate to provide an antibacterial and antiviral substrate. The appearance of the coated substrate is as follows. Figure 5 As shown.
[0133] Example 4
[0134] Production of antibacterial and antiviral masks and disposable gowns
[0135] The antibacterial and antiviral formulations of Examples 1-4 were sprayed onto face masks made of PP and disposable gowns made of PE, respectively. Products such as... Figure 6 As shown.
[0136] Example 5
[0137] Coating morphology of antibacterial and antiviral substrates
[0138] The coating morphology was evaluated using scanning electron microscopy. Antibacterial and antiviral substrates were cut into 1 cm x 1 cm pieces and placed on copper supports fitted with carbon ribbons. The samples were coated with gold for finishing. Figure 7 As shown, images from different locations on the sample were captured at different magnifications. Five samples from each embodiment were captured, and at least 100 pores of each sample were recorded. The average pore size was calculated by measuring the 100 pores of each sample.
[0139] Capture SEM images of antibacterial and antiviral substrates (e.g.) Figure 7 (As shown), and the pore size of the samples was measured by SEM. The average pore size (average of 100 pores) of 5 samples of bacterial and antiviral substrates is listed in Table 3 below.
[0140] Table 3
[0141] PP substrate (pore size, nanometer) PE substrate (pore size, nanometer) Sample 1 79 69 Sample 2 70 71 Sample 3 70 64 Sample 4 76 62 Sample 5 73 64 average: 74 66
[0142] Example 6
[0143] Physical properties of antibacterial and antiviral substrates
[0144] The physical performance evaluation of antibacterial and antiviral substrates includes particle filtration efficiency testing, air permeability testing, and moisture permeability testing.
[0145] PP and PE substrates were prepared for the following tests. The PP and PE substrates were the same as the antibacterial and antiviral substrates obtained in Example 3, but without the antibacterial and antiviral formulations.
[0146] In particle filtration efficiency (PFE) testing, the PALAS MFP 1000HPA filter testing system was used to test antibacterial and antiviral substrates (PP and PE), uncoated PP substrates, and uncoated PE substrates. Figure 8 As shown in the figure. Each sample was placed and fixed on the stage of the machine (top right figure). Particles ranging from 0.1 to 3 micrometers were generated by a testing machine containing a 2% sodium chloride solution and flowed through the test sample at a constant speed of 0.05 m / s for 1 minute. The sample test area was set to 0.01 square meters. The filtration efficiency was obtained by comparing the filtration results with the net particles flowing through the test chamber. 0.3 micrometer particles were used in the test because 0.3 micrometers is generally considered to be the most penetrating particle size (MPPS). The results are listed in Table 4.
[0147] Table 4
[0148]
[0149]
[0150] *: Another PP meltblown layer is coated on the substrate.
[0151] Antibacterial and antiviral PE substrates, as well as uncoated PE substrates, exhibited higher particle filtration efficiency. Both samples achieved particle filtration efficiencies exceeding 90%. Compared to the control group, the particle filtration efficiency of the antibacterial and antiviral PE substrates decreased by only 1.25%.
[0152] On the other hand, both the antibacterial and antiviral PP substrates and the uncoated PP substrates exhibited low particle filtration efficiency. The particle filtration efficiency of both samples was only slightly above 68%. Compared to the control group, the particle filtration efficiency of the antibacterial and antiviral PP substrates improved by 6.7%. After coating with the antibacterial and antiviral formulation of the present invention, the particle filtration efficiency of the PP and PE samples changed very little (i.e., less than 10%).
[0153] In the air permeability test, the FX 3360 portable air permeability tester was used to test antibacterial and antiviral PP substrates, antibacterial and antiviral PE substrates, uncoated PP substrates, and uncoated PE substrates. Figure 9 As shown in Table 5, aperture sizes of 20.7 mm and 0.5 mm were selected for measuring different material substrates to obtain suitable airflow and pressure (125 Pa) for the measurement. The test area for all substrates was fixed at 20 square centimeters. Air permeability was measured by the airflow passing through the test sample. The results are shown in Table 5.
[0154] Table 5
[0155]
[0156] Both the antibacterial and antiviral PP substrates and the uncoated PP substrates exhibited relatively high air permeability. The air permeability of both samples reached 380 cm⁻¹. 3 / cm 2 / s or higher. Compared to the control group, the air permeability of the antibacterial and antiviral PP substrate decreased by 2%. On the other hand, both the antibacterial and antiviral PE substrates and the uncoated PE substrate showed low air permeability. The air permeability of both samples was approximately 0.2 cm. 3 / cm 2 / s. Compared with the control group, the air permeability of the antibacterial and antiviral PE substrate decreased by 1.6%. After coating with the antibacterial and antiviral formulation of the present invention, both PP and PE samples met the requirement that the change in substrate air permeability was less than 10%.
[0157] In the moisture permeability test, the TF165B automatic water vapor permeability tester was used to test antibacterial and antiviral PP substrates, antibacterial and antiviral PE substrates, uncoated PP substrates, and uncoated PE substrates. Figure 10As shown. Before installing the sample substrate, 20 mL of water was first added to each permeation cup. Before placing the permeation cups in the test chamber (32℃, 50±2% humidity) for 24 hours, the weight of the permeation cups containing the sample substrate and water was recorded. After 24 hours, the weight of the permeation cups containing the sample substrate and remaining water was measured again, and the result was determined by the following... Figure 10 The equation in C calculates water vapor transmission rate (WVT): The results are shown in Table 6.
[0158] Table 6
[0159]
[0160] Both antibacterial and antiviral PP substrates and uncoated PP substrates exhibit high moisture permeability. The moisture permeability of both samples reached 120 g / h·m. 2 The above results indicate that the moisture permeability of the antibacterial and antiviral PP substrate decreased by 2.7% compared to the control group. On the other hand, both the antibacterial and antiviral PE substrates and the uncoated PE substrate exhibited relatively low moisture permeability. The moisture permeability of both samples reached 0.57 g / h·m. 2 The above is an overview. Compared to the control group, the moisture permeability of the antibacterial and antiviral PE substrate increased by 8.6%. After coating with the antibacterial and antiviral formulations of this invention, both PP and PE samples met the requirement that the change in moisture permeability of the substrate was less than 10%.
[0161] Example 7
[0162] Preparation of antibacterial and antiviral inks
[0163] Weigh 10 grams of the antibacterial and antiviral formulations from Examples 2-3 and add them to 90 grams of PU-based ink (thermosetting ink for screen printing and hot-melt ink for hot-melt printing). Add 0.1 grams of PHMB to the mixture and mix thoroughly. Store the resulting two antibacterial and antiviral inks separately in sealable containers, away from direct sunlight and heat sources.
[0164] Example 8
[0165] Preparation of antibacterial and antiviral substrates
[0166] Example 8-1
[0167] For screen printing, 100 grams of the antibacterial and antiviral thermosetting ink from Example 7 was loaded onto a screen with the designed printing pattern. The ink was rubbed from top to bottom onto the printed pattern on the screen to apply it to a 100% polyester substrate. This process was repeated 3 cycles to form a layer on the substrate for antimicrobial testing. The coated polyester substrate was then transferred to a 50°C oven for curing for 15 minutes to prepare the antibacterial and antiviral substrate. The screen printing process is as follows: Figure 11 As shown.
[0168] Example 8-2
[0169] For hot melt printing, the antibacterial and antiviral hot melt ink of Example 7 is loaded into the ink cartridge of an inkjet printer to print the designed pattern on heat transfer paper. The printed pattern on the heat transfer paper is allowed to cure. Hot melt powder is added to the pattern and heated at 180°C to form a hot melt layer. The heat transfer paper is then placed on a 100% polyester substrate on a hot press. The pattern is then heat-transferred onto the polyester substrate (e.g., ...). Figure 12 (as shown), and then an antibacterial and antiviral substrate is obtained.
[0170] Images of antibacterial and antiviral thermosetting inks, antibacterial and antiviral hot melt inks, and two types of antibacterial and antiviral substrates are shown below. Figure 13 As shown.
[0171] Example 9
[0172] Texture parameters of antibacterial and antiviral substrates
[0173] The polyester (PE) substrate was prepared for the following tests. The PE substrate was the same as the antibacterial and antiviral PE substrate, but without the antibacterial and antiviral formulation of Example 2.
[0174] like Figure 14A As shown, the texture parameters (hardness, bending, friction, and roughness) of antibacterial and antiviral PE substrates and uncoated PE substrates were measured using a fabric tactile tester.
[0175] The sample is cut into an L-shape and placed on the test stage of the fabric touch tester. The probe and probe are pulled into the machine. Texture parameters are recorded by the sensor.
[0176] The stiffness in the software (the degree to which it can withstand bending and compression to maintain its shape) is determined by... Figure 14C The term "compression" is shown. These parameters are affected by coating thickness and coating curing time. Parameters were measured on antibacterial and antiviral substrates as well as on polyester substrates, and recorded in Table 7. Compared to the control group, the changes in texture parameters (compression +8%, bending +10%, friction -1%, and roughness -7%) were less than 10%.
[0177] Table 7
[0178]
[0179]
[0180] Example 10
[0181] Inhibition Zone Test
[0182] Preliminary antimicrobial inhibition zone tests were performed on paper discs containing solution samples of the antibacterial and antiviral formulations of the present invention. Sterile paper discs with a diameter of 5 to 6 mm were placed on an agar surface inoculated with Staphylococcus aureus (0.1 mL of 10⁻⁶ oz). 6 Up to 10 7 (CFU / mL Staphylococcus aureus solution). Add 20 μL of the solution sample to a disc. Then incubate the agar plate in a 37°C incubator for at least 16 hours. If the test sample has antibacterial activity, a clear area will form. A clear area with a diameter greater than 1 mm indicates a positive antibacterial effect. The results of Examples 1 and 2 are described below.
[0183] Inhibition zone tests were performed on paper trays coated with the antibacterial and antiviral formulation of Example 1, revealing transparent areas (approximately 5 mm) (e.g.) Figure 15 As shown). An inhibition zone test was performed on the paper tray coated with the antibacterial and antiviral formulation of Example 2, and a transparent ring appeared (as shown). Figure 16 (As shown). Inhibition zone tests were performed on PP substrates coated with a 3-layer coating of the antibacterial and antiviral formulation of Example 1 and PP substrates coated with a 5-layer coating of the antibacterial and antiviral formulation of Example 1. The results are as follows. Figure 17 As shown.
[0184] Four samples of the antibacterial and antiviral PE substrate from Example 8-1 (freshly coated, 0-cycle washed, 5-cycle washed, and 10-cycle washed) were cut into 2 cm × 2 cm squares and placed on agar plates inoculated with Staphylococcus aureus (the freshly coated and 0-cycle washed samples were essentially the same). The agar plates containing the four samples were then incubated at 37°C for at least 16 hours (e.g., Figure 18 (As shown). Washing conditions (refer to AATCC 61, with additional wash time and additional drying process) are 40°C, washing for 1 hour with 2 grams of detergent (powder) from AATCC 1993 standard reference, followed by 1 hour of tumble drying at 60°C.
[0185] Example 11
[0186] Antibacterial and antiviral effects of PP substrate (SGS testing)
[0187] The antibacterial and antiviral effects of PP substrates were tested against Escherichia coli and Staphylococcus aureus according to the international standard ASTM E 2149-20. The tested substrates showed an antibacterial effect of over 99% against Escherichia coli and Staphylococcus aureus. The reduction value was calculated based on the comparison with the control group (Table 8).
[0188] Table 8
[0189]
[0190] Example 12
[0191] Antiviral properties of antibacterial and antiviral PP substrate (SGS testing)
[0192] The antiviral efficacy of the antimicrobial and antiviral PP substrate was tested according to the international standard ISO 18184:2019(E) for human coronavirus (HCoV-229E). The tested substrate showed an antiviral efficacy of over 99.99% against human coronavirus (Table 9).
[0193] Table 9
[0194]
[0195] Example 13
[0196] Antifungal properties of antibacterial and antiviral PP substrates (tested by Bureau Veritas).
[0197] The antifungal activity of antibacterial and antiviral PP substrates was tested according to the international standard ASTM G21-15, targeting *Azotomyces brasiliensis*, *Penicillium funiculosum*, *Chaetomium globosum*, *Trichoderma virens*, and *A. pullullans*. No tested fungi grew on the substrate surface (antifungal efficacy >99%) (Table 10).
[0198] It is worth noting that antiviral efficacy values are expressed in logarithmic decreases. For example, a logarithmic decrease of 2 indicates a 99% reduction, and a logarithmic decrease of 3 indicates a 99.9% reduction.
[0199] Table 10
[0200]
[0201] Example 14
[0202] Antimicrobial and antiviral properties of PP substrate against endospores (tested by Bureau Veritas).
[0203] The antimicrobial and antiviral activity of PP substrate against Bacillus subtilis was tested according to the international standard JIS Z 2801:2012. The obtained antimicrobial activity against Bacillus subtilis was a reduction in log [value missing]. 10 3.85, which indicates >99.9% resistance to endospores (Table 11).
[0204] Table 11
[0205] result: Bacillus subtilis <![CDATA[Logarithmic mean value of viable bacteria count (U0) immediately after inoculation of untreated test specimens]]> <![CDATA[Log 10 5.06]]> <![CDATA[Logarithmic mean value of viable bacteria count (U t ) after 24 hours of inoculation on untreated specimens <![CDATA[Log 10 4.85]]> <![CDATA[Logarithmic mean value of viable bacteria count (A t ) after 24 hours of inoculation on the substrate E1C-1 <![CDATA[Log 10 1.00]]> Antimicrobial activity (R) <![CDATA[Log 10 3.85]]>
[0206] Formula calculation: R = (U t -U0)–(A t -U0)
[0207] Example 15
[0208] Antibacterial properties of PE substrate coated with the antibacterial and antiviral formulation of this invention
[0209] The antimicrobial performance of polyester substrates coated with the antimicrobial and antiviral formulations of this invention was evaluated in vitro using an inhibition zone test. A plate method (refer to ASTM E 2149 or AATCC 100) was performed to assess microbial removal. Polyester substrates with and without the antimicrobial and antiviral formulation coatings were tested. 0.5 to 2 grams of coated or uncoated sample were added to a 250 mL Erlenmeyer flask containing 50 mL of Staphylococcus aureus solution at a concentration of 1.5 x 10⁻⁶. 5 -3x10 5 The bacterial solution was incubated at cfu / mL with shaking at 37°C for 18 to 24 hours. After incubation, the bacterial solution was diluted to different dilution factors and inoculated onto agar plates. The plates were incubated at 37°C for at least 16 hours. The bacterial colonies formed on the agar plates were counted and recorded. The percentage of bacterial removal was obtained by comparison with a blank control (uncoated PE substrate).
[0210] According to international standards, the antimicrobial and antiviral substrate of Example 8-1 was submitted to an accredited antimicrobial certificate holder. Antimicrobial tests were performed against *Escherichia coli* and *Staphylococcus aureus* (after 10 wash cycles), as per ASTM E 2149. Antispore tests against *Bacillus subtilis* were performed, as per JIS 2801. Antifungal tests were performed against 4 to 5 fungi, as per ASTM G21-15 or JIS Z 2911. Antiviral tests were performed against human coronaviruses, as per ISO 18184.
[0211] Example 16
[0212] Antiviral properties of antibacterial and antiviral PE substrates (SGS testing)
[0213] According to international standard ISO 18184:2019(E), the antiviral efficacy of the antimicrobial and antiviral PE substrate of Example 8-1 against human coronavirus (HCoV-229E) was tested in an accredited laboratory. The tested substrate showed 99.93% antiviral activity against human coronavirus (Table 12).
[0214] Table 12
[0215]
[0216] Example 17
[0217] Antibacterial and antiviral properties of PE substrates (tested by Bureau Veritas).
[0218] The antifungal activity of the antimicrobial and antiviral PE substrate was tested according to the international standard ASTM G21-15 in Example 8-1, targeting *Azotomyces brasiliensis*, *Penicillium funiculosum*, *Chaetomium globosum*, *Trichoderma virens*, and *A. pullullans*. No tested fungi grew on the substrate surface (antifungal efficacy >99%) (Table 13).
[0219] Table 13
[0220]
[0221] Growth observed on the sample Rating none 0 Minimal growth (less than 10%) 1 Mild growth (10-30%) 2 Moderate growth (30-60%) 3 Significant growth (60% full coverage) 4
[0222] Example 18
[0223] Antimicrobial and antiviral properties of PE substrates against endospores (tested by Bureau Veritas).
[0224] According to international standard JIS Z 2801:2012, the antimicrobial and antiviral PE substrate of Example 8-1 was tested for its antisporinogenic activity against Bacillus subtilis in an accredited laboratory. The obtained antisporinogenic effect was a reduction in log [value missing]. 10 3.26, which indicates an anti-endospore efficiency (endospore removal rate) of >99.9% (Table 14).
[0225] Table 14
[0226] result: Bacillus subtilis <![CDATA[Logarithmic mean value of viable bacteria count (U0) immediately after inoculation of untreated test piece]]> <![CDATA[Log 10 5.37]]> <![CDATA[Logarithmic mean value of viable bacteria count (U t ) after 24 hours of inoculation on untreated test pieces <![CDATA[Log 10 4.26]]> <![CDATA[Logarithmic mean value of viable bacteria count (A t )]]> <![CDATA[Log 10 1.00]]> Antimicrobial activity (R) <![CDATA[Log 10 3.26]]>
[0227] Formula calculation: R = (U t -U0)–(A t -U0)
[0228] Example 19
[0229] Wash resistance of antibacterial and antiviral polyester substrates
[0230] Wash the polyester substrate coated with the antibacterial and antiviral formulation of Example 2 according to international standards such as AATCC 61A1. The washing conditions for AATCC 61 are shown in Table 15. 0.37 g of laundry detergent was added to 200 ml of water containing 10 steel balls, and the coated substrate was washed at 40°C for 45 minutes. The antibacterial effect was evaluated after 5 and 10 wash cycles, and the results are as follows: Figure 18 As shown in Table 15.
[0231] Table 15
[0232]
[0233] Antimicrobial effect of coated polyester substrate after 10 washing cycles (e.g., ASTM E 2149) according to industry standards (e.g., ASTM E3162-18).
[0234] According to the international standard ASTM E 2149, the antibacterial effect of the coated polyester substrate after 10 washing cycles under AATCC 61A1 conditions was tested using Escherichia coli and Staphylococcus aureus. The results are shown in Table 16. The obtained antibacterial effects against both Escherichia coli and Staphylococcus aureus were greater than 99%.
[0235] Table 16
[0236]
[0237] According to the international standard ASTM E 2149, after 10 washing cycles, the coated polyester substrate was tested by Bureau Veritas to obtain additional verification of its antimicrobial properties.
[0238] Table 17
[0239]
[0240] Note: Reduction percentage (%) = [(CA) / C)] x 100%
[0241] The antimicrobial and antiviral formulations of Examples 1-4 (Group 1) and Examples 2-3 (Group 2), the antimicrobial and antiviral PP substrates (Group 3) and PE substrates (Group 4), and the antimicrobial and antiviral PE substrate of Example 8-1 (Group 5) were tested in an accredited third-party laboratory to assess chemical and biological safety. The results are shown in Table 18.
[0242] Table 18
[0243]
[0244]
[0245] *RoHS & SVHC are conducted by Intertek Testing Services HK Ltd.
[0246] USP 467 was conducted at Jialigao Testing Center Co., Ltd.
[0247] ***Skin irritation and acute skin toxicity tests were conducted by SGS.
[0248] The antimicrobial and antiviral formulations were tested for hazardous substances restricted or prohibited under RoHS and SVHC. The levels of the detected substances did not exceed permissible limits. The VOC content of the antimicrobial and antiviral formulations was tested according to USP 467 (Class 1 Residual Solvents). The detected residual solvents did not exceed permissible limits. Skin irritation of the antimicrobial and antiviral substrates to patient skin was tested using test patches. The testing methods followed the in-house methods of an accredited testing laboratory. No irritation was observed or was negligible. Acute contact toxicity testing was performed on the antimicrobial and antiviral substrates to provide information on potential health hazards from short-term skin contact with the chemicals. No acute contact toxicity was observed or was negligible.
[0249] definition
[0250] Throughout this specification, unless otherwise specified, the term "comprising" or variations thereof will be understood to include a specified whole or entirety, but does not exclude the inclusion of any other whole or group of wholes. It should also be noted that in this disclosure, particularly in the claims or during the period, the terms "comprising" or "comprising" have the meaning given to them under U.S. patent law. For example, they allow for undefined elements but exclude elements found in the prior art or affecting the essential or novel features of the invention.
[0251] Furthermore, throughout the specification and claims, unless otherwise required, the term "comprising" or variations thereof shall be understood to include a specified whole or group of wholes, but not to exclude the inclusion of any other whole or group of wholes.
[0252] As used herein, the terms "substantially," "essentially," "approximately," and "about" are used to describe and explain a small variation. When used in conjunction with an event or situation, the term can refer to the exact occurrence of the event or situation, or to an approximate occurrence. For example, when used with numerical values, these terms can encompass a range of variation less than or equal to ±10% of the numerical value, such as less than or equal to ±5%, less than or equal to ±4%, less than or equal to ±3%, less than or equal to ±2%, less than or equal to ±1%, less than or equal to ±0.5%, less than or equal to ±0.1%, or less than or equal to ±0.05%.
[0253] The specification uses terms such as "an embodiment," "embodiment," and "example embodiment" to indicate that the described embodiment may include specific features, structures, or characteristics. However, each embodiment need not include these specific features, and these features do not necessarily refer to the same embodiment. Furthermore, when a specific feature, structure, or characteristic is described in conjunction with an embodiment, it is assumed that it is within the knowledge of those skilled in the art, and whether explicitly described or not, these features, structures, or characteristics can be applied in conjunction with other embodiments.
[0254] In the preparation methods described herein, the steps may be performed in any order without departing from the principles of the invention, unless the temporal or operational order is explicitly stated. In a claim, it should be stated that one step is performed before several other steps, meaning the first step is performed before any other steps, but the other steps may be performed in any suitable order unless the sequence is further enumerated in the other steps. For example, a claim element enumerating "steps A, B, C, D, and E" should be understood to mean that step A is performed first and step E is performed last, and steps B, C, and D may be performed in any order between steps A and E, and this order remains within the literal scope of the claim process. A given step or subset of steps may also be repeated.
[0255] Other definitions of alternative terms used herein can be found in the detailed description of the invention and applied throughout. Unless otherwise defined, all other technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.
Claims
1. An antibacterial and antiviral fabric, characterized in that, include: A fabric substrate; At least one antimicrobial coating formed on the fabric substrate, the antimicrobial coating comprising an antimicrobial agent having at least two antimicrobial components, which is embedded or surface-adhered in a three-dimensional porous network of nano-adhesive particles, wherein the three-dimensional porous network is formed by interconnecting the nano-adhesive particles through van der Waals forces or Coulomb forces. The nano-binder particles comprise chitosan, zein, at least one organic binder selected from gelatin, cellulose, alginate, pectin, acrylic latex, polyurethane, or cyclodextrin, and at least one inorganic solid particle component selected from silica or zinc oxide; and The antibacterial and antiviral fabrics described herein have an antibacterial effect of at least 99% while retaining physical properties comparable to uncoated fabrics.
2. The antibacterial and antiviral fabric according to claim 1, wherein the three-dimensional porous network has pores surrounded by the nano-adhesive particles, and the average pore size of the three-dimensional porous network is at least 50 nanometers.
3. The antimicrobial and antiviral fabric according to claim 1, wherein the antimicrobial agent is embedded or surface-adhered to the nano-adhesive particles to form antimicrobial and antiviral nanoparticles having a particle size of 100 nanometers to 800 nanometers.
4. The antibacterial and antiviral fabric according to claim 3, wherein the antibacterial and antiviral nanoparticles have a polydispersity of 0.05 to 0.
5.
5. The antibacterial and antiviral fabric according to claim 1, wherein the fabric substrate is selected from one or more of the following: polypropylene (PP) substrate, polyethylene (PE) substrate, polyester substrate, cotton substrate, nylon, spandex substrate, cotton-polyester blend, cotton-nylon blend, and cotton-spandex blend.
6. The antimicrobial and antiviral fabric according to claim 1, wherein the at least two antimicrobial components are selected from two or more of polyhexamethylene biguanide, chlorhexidine, zinc pyrithione, gallic acid, nisin, and silane quaternary ammonium compounds.
7. The antibacterial and antiviral fabric according to claim 1, wherein the antibacterial and antiviral fabric is breathable, with a surface area increased by at least 1000% and porosity increased by at least 1000%.
8. An antibacterial and antiviral formulation for soft surfaces, characterized in that, include: Antimicrobial agent, 0.01% to 5% by weight; Nano-binder particles, ranging from 0.01% to 5% by weight; Surfactants and solvents; The antimicrobial agent comprises a combination of chlorhexidine and polyhexamethylene biguanide; the nano-binder particles comprise chitosan, zein, and zinc oxide, which synergistically construct a three-dimensional nanonetwork.
9. The antibacterial and antiviral formulation according to claim 8, wherein the surfactant is used in an amount of 0.01% to 10% by weight, and the solvent is used in an amount of 85.0% to 99.5% by weight.
10. The antibacterial and antiviral formulation according to claim 8, wherein the antibacterial and antiviral formulation further comprises a crosslinking agent selected from the group consisting of: tripolyphosphate (TPP), glutaraldehyde, critical acid, adipic acid, 1,2,3,4-butanedicarboxylic acid (BTCA), methoxy polyethylene glycol aldehyde, and dimethyloldihydroxyethylene urea, wherein the crosslinking agent is used in an amount of 0.01% to 1% by weight.
11. The antibacterial and antiviral formulation according to claim 8, wherein the solvent comprises a first solution and a second solution; the first solution is selected from water, ethyl acetate, isopropanol, ethanol, acetic acid, ammonia or combinations thereof, the second solution is selected from isopropyl myristate (IPM), isopropyl palmitate, oleic acid, almond oil, soybean oil or combinations thereof, and the surfactant is selected from cetrimonium bromide (CTAB), polysorbate 20, polysorbate 80, sorbitol laurate, sorbitol oleate, polyglycerol-6 caprylate, polyglycerol-3-cocoate, polyglycerol-4-decanoate, polyglycerol-6-ricinoleate or combinations thereof.
12. The antibacterial and antiviral formulation according to claim 11, wherein the surfactant is used in an amount of 0.01% to 10% by weight, the first solution is used in an amount of 85.0% to 99.5% by weight, and the second solution is used in an amount of 0.01% to 5% by weight.
13. A method for preparing antibacterial and antiviral nanoparticles, characterized in that, include: Step (a) provides a first mixture comprising at least one antimicrobial component and at least one adhesive component; Step (b) homogenizes the first mixture; and Step (c) involves adding at least one other antimicrobial ingredient and at least one other binder ingredient, and mixing them with the first mixture to form a second mixture, wherein the antibacterial and antiviral nanoparticles are formed in the second mixture; Wherein, based on the weight of the second mixture, the content of the antimicrobial component is 0.01% to 5% by weight, and the content of the adhesive component is 0.01% to 5% by weight. The antimicrobial component is embedded in or adhered to the surface of the nano-adhesive particles to form the antibacterial and antiviral nanoparticles. The nano-adhesive particles include chitosan, zein, and zinc oxide, which synergistically construct a three-dimensional nanonetwork.
14. The method of claim 13, wherein the pressure in step (b) is in the range of 0 bar to 1000 bar.
15. The method of claim 13, wherein the pressure in step (b) is in the range of 200 bar to 700 bar.
16. The method of claim 13, wherein step (a) or step (c) further comprises adding a surfactant in an amount of 0.01 to 10% by weight and a solvent in an amount of 85.0% to 99.5% by weight.
17. The method of claim 13, wherein step (b) further comprises a heat treatment step at 40°C to 70°C.
18. The method of claim 13, wherein the antimicrobial component comprises polyhexamethylene biguanide, chlorhexidine, zinc pyrithione, gallic acid, nisin, or a silane quaternary ammonium compound; and the adhesive component comprises chitosan, zein, at least one organic adhesive selected from gelatin, cellulose, alginate, pectin, acrylic latex, polyurethane, or cyclodextrin, and at least one inorganic component selected from silicon dioxide, zinc oxide, titanium dioxide, copper oxide, or iron oxide.
Citation Information
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