An antibacterial antiviral agent, its method of preparation and use in sanitizing wipes

Abstract

The application discloses an antibacterial and antiviral agent, which comprises the following components in parts by weight: 100 parts of water, 0.04-0.1 parts of cetylpyridinium chloride, 0.2-0.6 parts of benzalkonium chloride, 0.1-0.3 parts of polyhexamethylene biguanide hydrochloride, 0.04-0.16 parts of phenoxyethanol, 0.5-5 parts of silica-supported metal silver nanoparticles, 0.4-1.0 parts of propylene glycol, 0.02-0.06 parts of glycerol and 0.02-0.06 parts of EDTA-2Na. The application further discloses a preparation method of the antibacterial and antiviral agent. The antibacterial and antiviral agent provided by the application can synergistically enhance the effect by compounding cetylpyridinium chloride, benzalkonium chloride, polyhexamethylene biguanide hydrochloride and silica-supported metal silver nanoparticles, reduces the active ingredients such as cetylpyridinium chloride and benzalkonium chloride, and maintains excellent bactericidal effect; and the combination of silica-supported metal silver nanoparticles with different particle sizes enables the sanitary wet wipe liquid to not only quickly kill bacteria but also kill bacteria for a long time, and effectively improves the bactericidal efficiency and bactericidal timeliness of the sanitary wet wipe liquid.

Description

Technical Field

[0001] This invention belongs to the field of daily chemical products technology, specifically relating to an antibacterial and antiviral agent, its preparation method, and its application in disinfectant wipes. Background Technology

[0002] As a convenient and efficient cleaning and hygiene product, wet wipes are widely used in personal care and daily disinfection. With the general increase in public health awareness and the need for routine prevention and control of infectious diseases, the market's perception of wet wipes has gradually shifted from basic cleaning to a multi-functional approach that combines protection, safety, and long-lasting effectiveness. Currently, wet wipes with safe and long-lasting anti-pathogen capabilities are becoming an important part of personal and public hygiene protection.

[0003] However, commercially available wet wipes currently face significant limitations in achieving antibacterial and antiviral functions: 1) Most products rely on traditional chemical bactericidal ingredients (such as alcohol, quaternary ammonium salts, triclosan, etc.), and to achieve a good bactericidal effect, the content is generally high, which can easily lead to skin irritation with long-term use; 2) Existing products have excellent bactericidal effects, but poor long-lasting effects, resulting in the need for frequent use in actual applications; 3) Existing products generally lack systematic verification of their effectiveness and safety against specific common pathogens. In particular, for highly infectious pathogens such as influenza A virus, human papillomavirus (HPV), hand-foot-and-mouth disease-related viruses, pneumonia pathogens, and norovirus, their inhibition and clearance effects lack reliable experimental data, making it difficult to provide stable protection in real-world usage scenarios.

[0004] Therefore, developing a specialized antibacterial composition for wet wipes that combines broad-spectrum antiviral and antibacterial properties with mild safety and long-lasting antibacterial effects is of significant practical importance. This composition should undergo scientific in vitro and simulated experiments to verify its antipathogenic effects, while also considering user comfort, skin care functions, and material safety. This will meet consumers' dual needs for effective protection and health care, and drive the wet wipes industry towards a safer, more professional, and functional direction. Summary of the Invention

[0005] This invention aims to at least partially solve one of the technical problems in related technologies. Therefore, the main objective of this invention is to provide an antibacterial and antiviral agent, its preparation method, and its application in disinfectant wipes.

[0006] The objective of this invention is achieved through the following technical solution:

[0007] An antibacterial and antiviral agent comprising, by weight, the following components: 100 parts water, 0.04-0.1 parts cetylpyridinium chloride, 0.2-0.6 parts benzalkonium chloride, 0.1-0.3 parts polyhexamethylene biguanide hydrochloride, 0.04-0.16 parts phenoxyethanol, 0.5-3 parts silica-supported silver nanoparticles, 0.4-1.0 parts propylene glycol, 0.02-0.06 parts glycerol, and 0.02-0.06 parts EDTA-2Na (disodium ethylenediaminetetraacetate).

[0008] In some specific embodiments, the silica-supported silver nanoparticles are a mixture of silica-supported silver nanoparticles with a particle size of 20-50 nm and silica-supported silver nanoparticles with a particle size of 100-300 nm, with a mass ratio of 1:(2-5).

[0009] In some specific embodiments, the silica-supported silver nanoparticles are obtained by the following preparation method:

[0010] 1) Disperse nano-silica microspheres in ethanol / water solution, adjust the pH of the reaction system to 4-5, and after ultrasonic dispersion, add γ-mercaptopropyltrimethoxysilane for grafting reaction, centrifuge and wash to obtain modified nano-silica microspheres.

[0011] 2) Dissolve the modified nano-silica microspheres from step 1) in deionized water, then add silver nitrate solution, stir evenly, and then add L-ascorbic acid solution dropwise to carry out the reduction reaction. Centrifuge the reduction product to obtain the reaction product, wash and dry the reaction product to obtain silica-loaded silver nanoparticles.

[0012] The ethanol / aqueous solution is a mixture of ethanol and deionized water in a mass ratio of 3:1; the pH of the reaction system is adjusted by glacial acetic acid.

[0013] In some specific embodiments, the process conditions for the grafting reaction in step 1) are: reacting in a water bath at 60-80°C for 4-8 hours.

[0014] In some specific embodiments, the mass ratio of the nano-silica microspheres and γ-mercaptopropyltrimethoxysilane in step 1) is (5-15):(0.5-5).

[0015] In some specific embodiments, the modified nano-silica microspheres described in step 2) have a mass ratio of silver nitrate and L-ascorbic acid of (5-15):(0.3-1.0):(0.1-0.6).

[0016] In some specific embodiments, the reduction reaction in step 2) is carried out under the following process conditions: at a pH of 7.0-8.0, the reaction is carried out at 40-80°C for 1-3 hours.

[0017] As part of the same inventive concept, this invention also provides a method for preparing the aforementioned antibacterial and antiviral agent, comprising the following steps:

[0018] S1. Weigh an appropriate amount of purified water and add it to the mixing tank. Set the temperature to 50-60℃. Then add the weighed cetylpyridinium chloride, benzalkonium chloride, polyhexamethylene biguanide hydrochloride, and EDTA-2Na to the purified water in sequence to form a complex. Stir and disperse the mixture evenly at a speed of 50-150 rpm. Keep the temperature at 50-60℃ for 30-45 minutes.

[0019] S2. Turn off the heating system, turn on the stirrer to cool naturally. When the temperature of the composite material drops below 40℃, slowly add phenoxyethanol, propylene glycol and glycerin in sequence. Stir evenly, then add silica-supported silver nanoparticles and continue stirring until evenly dispersed. Turn off the stirrer, take a sample for testing and discharge after it passes the test.

[0020] As part of the same inventive concept, the present invention also provides a disinfecting wipe, comprising a non-woven fabric substrate and a sanitary wipe liquid, characterized in that the sanitary wipe liquid comprises the aforementioned antibacterial and antiviral agents.

[0021] Compared with the prior art, the present invention has at least the following advantages:

[0022] 1) The antibacterial and antiviral agent provided by the present invention can achieve synergistic effects by compounding cetylpyridinium chloride, benzalkonium chloride, polyhexamethylene biguanide hydrochloride and silica-loaded silver nanoparticles. While maintaining the bactericidal effect, it greatly reduces the use of active ingredients such as cetylpyridinium chloride and benzalkonium chloride, thereby reducing irritation to the skin or the user and improving the safety and gentleness of the sanitary wipe liquid.

[0023] 2) The silica-loaded silver nanoparticles of the present invention are prepared by modifying the nano-silica microspheres with γ-mercaptopropyltrimethoxysilane and then partially reducing the silver nitrate solution with L-ascorbic acid. When the silica-loaded silver nanoparticles are used in antibacterial and antiviral agents, they not only effectively improve the stability of the sanitary wipes, but also give the sanitary wipes a sustained-release function, thus effectively improving the long-term stability of the sanitary wipes.

[0024] 3) This invention employs silica-loaded silver nanoparticles of different particle sizes for composite composition, combined with active ingredients such as cetylpyridinium chloride and benzalkonium chloride. In practical use, cetylpyridinium chloride and benzalkonium chloride in the sanitary wipe liquid can quickly adsorb and destroy bacterial cell membranes, thereby achieving efficient and rapid sterilization. At the same time, the small-particle-size silica-loaded silver nanoparticles can rapidly diffuse to the surrounding area of ​​bacteria that have been destroyed by cetylpyridinium chloride and benzalkonium chloride, penetrating deep into the cells for secondary sterilization, synergistically enhancing the bactericidal effect of the antibacterial and antiviral agent. Meanwhile, the large-particle-size silica-loaded silver nanoparticles effectively improve the bactericidal timeliness of the antibacterial and antiviral agent, indicating that the large-particle-size silica-loaded silver nanoparticles achieve a sustained-release effect in the antibacterial and antiviral agent, exhibiting a good long-lasting antibacterial effect. This product combines active ingredients such as cetylpyridinium chloride and benzalkonium chloride with silica-loaded silver nanoparticles of different particle sizes, enabling the sanitary wipes to not only kill bacteria quickly but also to kill bacteria for a long time, effectively improving the sterilization efficiency and duration of the sanitary wipes. Detailed Implementation

[0025] The present invention will be further described in detail below with reference to specific embodiments. The following embodiments are merely descriptive and not limiting, and should not be used to limit the scope of protection of the present invention.

[0026] When a quantity, concentration, or other value or parameter is described as a range, preferred range, or preferred upper and lower limits, it should be understood that it is equivalent to specifically disclosing any range by combining any pair of upper or preferred values ​​with any lower or preferred values, regardless of whether the range is specifically disclosed. Unless otherwise stated, the numerical range values ​​listed herein include the endpoints of the range and all integers and fractions within that range.

[0027] Unless otherwise stated, all percentages, parts, ratios, etc. in this document are by weight.

[0028] The materials, methods, and embodiments described herein are exemplary and should not be construed as limiting unless otherwise stated.

[0029] This invention provides a general and / or specific description of the materials and experimental methods used in the experiments. Unless otherwise specified, all experimental or testing methods are conventional methods; all reagents or instruments used, unless otherwise specified, are commercially available conventional products prepared or used using conventional methods.

[0030] Example 1

[0031] This embodiment provides a method for preparing silica-supported silver nanoparticles, which includes the following steps:

[0032] 1) Disperse 15 parts by weight of nano-silica microspheres (SiO2, the same below) with a particle size of 20-50nm (or 100-300nm) in a mixed solution of ethanol and deionized water with a mass ratio of 3:1. At the same time, adjust the pH value of the reaction system to 4-5 with glacial acetic acid. Sonicate for 30 min to ensure full dispersion. Under continuous stirring, slowly add 0.5 parts by weight of γ-mercaptopropyltrimethoxysilane (KH590) to the above dispersion. After mixing evenly, react in a 60℃ water bath for 6 h to successfully graft silane onto the SiO2 surface. Centrifuge the product at 1500 rpm for 2 min and wash it twice with ethanol to obtain modified nano-silica microspheres.

[0033] 2) Dissolve 12 parts by weight of the modified nano-silica microspheres from step 1) in 200 parts by weight of deionized water, then add silver nitrate solution, followed by 0.5 parts by weight of silver nitrate solution. Stir at room temperature for 1 hour to obtain a mixture. Add 0.5 parts by weight of L-ascorbic acid solution dropwise to the mixture and adjust the pH to 8.0 with 25% concentrated ammonia. Stir the reaction at 60°C for 1 hour. Centrifuge the reduction product at 5000 rpm for 15 minutes, discard the supernatant to obtain the reaction product. Wash the reaction product three times with deionized water by centrifugation. Freeze-dry the obtained solid product for 24 hours to obtain silica-supported silver nanoparticles with a particle size of 20-50 nm (or 100-300 nm).

[0034] The preparation method for silica-supported silver nanoparticles with a particle size of 100-300 nm is the same as that for silica-supported silver nanoparticles with a particle size of 20-50 nm.

[0035] Example 2

[0036] This embodiment provides a method for preparing an antibacterial and antiviral agent, comprising the following steps:

[0037] S1. Weigh 100 parts (all by weight, the same below) of purified water and add it to the mixing tank. Set the temperature to 50℃. Then add 0.02 parts of cetylpyridinium chloride, 0.3 parts of benzalkonium chloride, 0.05 parts of polyhexamethylene biguanide hydrochloride, and 0.02 parts of EDTA-2Na to the purified water in sequence to form a complex. Stir and disperse evenly at 100 rpm. Raise the temperature to 55℃ and keep it warm for 30 min.

[0038] S2. Turn off the heating system, turn on the stirrer and let it cool naturally. When the temperature of the composite material drops below 40℃, slowly add 0.05 parts phenoxyethanol, 0.3 parts propylene glycol and 0.02 parts glycerol in sequence. After stirring evenly, add 3 parts silica-supported silver nanoparticles (the mass ratio of silica-supported silver nanoparticles with a particle size of 20-50nm to silica-supported silver nanoparticles with a particle size of 100-300nm is 1:2). Continue stirring until it is evenly dispersed. Turn off the stirrer, take a sample and test it. After it passes the test, discharge the material.

[0039] Example 3

[0040] This embodiment provides a method for preparing an antibacterial and antiviral agent, comprising the following steps:

[0041] S1. Weigh 100 parts (all by weight, the same below) of purified water and add it to the mixing tank. Set the temperature to 55℃. Then add 0.03 parts of cetylpyridinium chloride, 0.2 parts of benzalkonium chloride, 0.1 parts of polyhexamethylene biguanide hydrochloride, and 0.02 parts of EDTA-2Na to the purified water in sequence to form a complex. Stir and disperse evenly at 100 rpm. Raise the temperature to 60℃ and keep it warm for 30 min.

[0042] S2. Turn off the heating system, turn on the stirrer and let it cool naturally. When the temperature of the composite material drops below 40℃, slowly add 0.05 parts phenoxyethanol, 0.3 parts propylene glycol and 0.02 parts glycerol in sequence. After stirring evenly, add 2 parts silica-supported silver nanoparticles (the mass ratio of silica-supported silver nanoparticles with a particle size of 20-50nm to silica-supported silver nanoparticles with a particle size of 100-300nm is 1:3). Continue stirring until it is evenly dispersed. Turn off the stirrer, take a sample and test it. After it passes the test, discharge the material.

[0043] Example 4

[0044] This embodiment provides a method for preparing an antibacterial and antiviral agent, comprising the following steps:

[0045] S1. Weigh 100 parts (all by weight, the same below) of purified water and add it to the mixing tank. Set the temperature to 50℃. Then add 0.05 parts of cetylpyridinium chloride, 0.1 parts of benzalkonium chloride, 0.15 parts of polyhexamethylene biguanide hydrochloride, and 0.02 parts of EDTA-2Na to the purified water in sequence to form a complex. Stir and disperse evenly at 100 rpm. Raise the temperature to 55℃ and keep warm for 45 min.

[0046] S2. Turn off the heating system, turn on the stirrer and let it cool naturally. When the temperature of the composite material drops below 40℃, slowly add 0.05 parts phenoxyethanol, 0.3 parts propylene glycol and 0.02 parts glycerol in sequence. Stir evenly, then add 1 part silica-supported silver nanoparticles (the mass ratio of silica-supported silver nanoparticles with a particle size of 20-50nm to silica-supported silver nanoparticles with a particle size of 100-300nm is 1:4). Continue stirring until evenly dispersed, turn off the stirrer, take a sample and test it. After passing the test, discharge the material.

[0047] Comparative Example 1

[0048] This embodiment provides a method for preparing an antibacterial and antiviral agent, the process steps and parameters of which are the same as in Example 3; the components and proportions are basically the same as in Example 3, the difference being that the modifier in step 1) of the method for preparing silica-supported silver nanoparticles (Example 1) is γ-aminopropyltriethoxysilane (KH560), the specific steps of which are as follows:

[0049] 1) Disperse 15 parts by weight of nano-silica microspheres with a particle size of 20-50 nm (or 100-300 nm) in a mixed solution of 200 parts by weight of ethanol and deionized water with a mass ratio of 3:1. At the same time, adjust the pH value of the reaction system to 4-5 with glacial acetic acid. Sonicate for 30 min to ensure full dispersion. Under continuous stirring, slowly add 0.5 parts by weight of γ-aminopropyltriethoxysilane to the above dispersion. After mixing evenly, react in a 60℃ water bath for 6 h to successfully graft silane onto the SiO2 surface. Centrifuge the product at 1500 rpm for 2 min and wash it twice with ethanol to obtain modified nano-silica microspheres.

[0050] Step 2) is the same as in Example 1;

[0051] The preparation method for silica-supported silver nanoparticles with a particle size of 100-300 nm is the same as that for silica-supported silver nanoparticles with a particle size of 20-50 nm.

[0052] Comparative Example 2

[0053] This embodiment provides a method for preparing an antibacterial and antiviral agent. The process steps and parameters are the same as in Example 3, and the components and ratios are basically the same. The only difference is that in the preparation method of silica-supported silver nanoparticles (Example 1), the reducing agent in step 2) is a sodium citrate solution, and the corresponding ratios and reaction conditions are suitable for the sodium citrate system. Specifically:

[0054] 1) Same as Example 1;

[0055] 2) Dissolve 12 parts by weight of the modified nano-silica microspheres from step 1) in 200 parts by weight of deionized water, then add 0.5 parts by weight of silver nitrate solution, stir at room temperature for 1 h to obtain a mixture, add 1.2 parts by weight of sodium citrate solution dropwise to the mixture, reflux and stir at 100℃ boiling temperature for 1.5 h, centrifuge the reduction product at 5000 rpm for 15 min, discard the supernatant to obtain the reaction product, wash the reaction product three times with deionized water by centrifugation, freeze-dry the obtained solid product for 24 h to obtain silica-supported silver nanoparticles with a particle size of 20-50 nm (or 100-300 nm);

[0056] The preparation method for silica-supported silver nanoparticles with a particle size of 100-300 nm is the same as that for silica-supported silver nanoparticles with a particle size of 20-50 nm.

[0057] Comparative Example 3

[0058] This embodiment provides a method for preparing an antibacterial and antiviral agent. The process steps and parameters are the same as in Example 3, and the components and ratios are basically the same. The only difference is that in the preparation method of silica-supported silver nanoparticles (Example 1), the reducing agent in step 2) is sodium borohydride solution, and the corresponding ratios and reaction conditions are suitable for a sodium citrate system. Specifically:

[0059] 1) Same as Example 1;

[0060] 2) Dissolve 12 parts by weight of the modified nano-silica microspheres from step 1) in 200 parts by weight of deionized water, then add 0.5 parts by weight of silver nitrate solution, stir at room temperature for 1 h to obtain a mixture, add 0.3 parts by weight of sodium borohydride solution dropwise to the mixture, react in an ice-water bath at 0℃ for 1 h, centrifuge the reduction product at 5000 rpm for 15 min, discard the supernatant to obtain the reaction product, wash the reaction product three times with deionized water by centrifugation, freeze-dry the obtained solid product for 24 h to obtain silica-supported silver nanoparticles with a particle size of 20-50 nm (or 100-300 nm);

[0061] The preparation method for silica-supported silver nanoparticles with a particle size of 100-300 nm is the same as that for silica-supported silver nanoparticles with a particle size of 20-50 nm.

[0062] Comparative Example 4

[0063] This comparative example provides a method for preparing an antibacterial and antiviral agent. The process steps and parameters are the same as those in Example 3, and the components and ratios are basically the same as those in Example 3. The difference is that only silica-supported silver nanoparticles with a particle size of 20-50 nm are added.

[0064] Comparative Example 5

[0065] This comparative example provides a method for preparing an antibacterial and antiviral agent. The process steps and parameters are the same as those in Example 3, and the components and ratios are basically the same as those in Example 3. The difference is that only silica-supported silver nanoparticles with a particle size of 100-300 nm are added.

[0066] Comparative Example 6

[0067] This comparative example provides a method for preparing an antibacterial and antiviral agent. The process steps and parameters are the same as those in Example 3, and the components and ratios are basically the same as those in Example 3. The difference is that silica-supported silver nanoparticles are not added.

[0068] Performance testing:

[0069] Test Example 1: Stability of Antibacterial and Antiviral Agents

[0070] This application uses Example 3 as an example to illustrate the antibacterial and antiviral agents in Example 3 and Comparative Examples 1-6.

[0071] The stability test lasted for one month (the stock solution was tested at 4°C, room temperature, 55°C, and a 0.5% aqueous solution at room temperature). The experimental results are shown in Table 1.

[0072] Table 1. Stability of antibacterial and antiviral agents in Example 3 and each comparative example.

[0073]

[0074] The data in the table show that the antibacterial and antiviral agent provided by this invention has excellent stability. A comparison of Example 3 with Comparative Examples 1 and 2 reveals that the types of modifiers and reducing agents used in the silica-supported silver nanoparticles of this application have a significant impact on their stability in the antibacterial and antiviral agent. This is likely because, in the antibacterial and antiviral agent system, the γ-mercaptopropyltrimethoxysilane and Ag in the silica-supported silver nanoparticles of this application… + Ions form stable Ag + -S coordinate bonds effectively reduce free Ag. + This reduces free Ag + Cl in antibacterial and antiviral agents - It can form a precipitate or crystals.

[0075] Since the antibacterial and antiviral agents prepared in Comparative Examples 1, 2, and 3 failed to meet the technical requirements in terms of stability, no further tests were conducted.

[0076] Test Example 2: Time-Effect Test of Antibacterial and Antiviral Agents

[0077] 1) Neutralizer identification test

[0078] Test samples: Antibacterial and antiviral agents prepared in Example 3 and Comparative Examples 4-6;

[0079] Test Methods: The indicator bacteria for the neutralizing agent identification test were Escherichia coli and Staphylococcus aureus. Six groups of tests were designed, and the neutralizing agent identification test was conducted according to the quantitative bactericidal suspension test procedure. The test operation procedures and result judgment criteria were all carried out in accordance with the provisions of the 2002 edition of the "Disinfection Technical Specifications".

[0080] Test reagents: Phosphate-buffered saline (PBS) containing 5 g / L sodium thiosulfate and 0.5 g / L Tween 80 was used as a neutralizing agent;

[0081] Test results: The neutralizing agent can effectively neutralize the residual effects of the antibacterial and antiviral agents prepared in Example 3 and Comparative Examples 4-6 on Escherichia coli and Staphylococcus aureus at the highest test concentration; and the neutralizing agent and neutralization product are non-toxic to the tested microorganisms and meet the specified requirements.

[0082] 2) Sterilization / bacteriostatic performance test

[0083] Test method: The quantitative bactericidal test of suspension was conducted at room temperature;

[0084] Test samples: Antibacterial and antiviral agents prepared in Example 3 and Comparative Examples 4-6

[0085] Preparation of bacterial suspension: Staphylococcus aureus was isolated and purified, inoculated onto ordinary nutrient agar slant, and cultured at 37°C for 24 hours; the fresh slant culture was taken, washed down with physiological saline and diluted to prepare bacterial suspension; during the experiment, the bacterial suspension was diluted with organic interfering substances by a factor of 2 to prepare the bacterial suspension of the test concentration for later use.

[0086] Bactericidal efficiency test: At room temperature (25℃), 60 μL of bacterial suspension was added to 240 μL of antibacterial and antiviral agent, mixed well, and allowed to act for 15 s, 30 s, 2 min, 5 min, and 8 min. Then, 20 μL of the mixture was added to 180 μL of neutralization solution (PBS containing 5 g / L sodium thiosulfate and 0.5 g / L Tween 80) for 5 min to terminate the reaction. 50 μL of the sample solution was placed on a nutrient agar plate, spread evenly with a sterile L-shaped rod, and incubated at 37℃ for 24 h. Colony counting was performed. The test was repeated three times, and the average kill rate (logarithmic sterilization value after action time) was calculated. The test results are shown in Table 2.

[0087] Table 2. Test results of bactericidal and antiviral properties of the antibacterial and antiviral agents in Example 3.

[0088]

[0089] As can be seen from the data in Table 2, the antibacterial and antiviral agent provided by the present invention has excellent bactericidal efficiency and bactericidal effect.

[0090] Long-term effectiveness test: At room temperature (25℃), 60 μL of bacterial suspension was added to 240 μL of antibacterial and antiviral agent, mixed well, and allowed to act for 3 h and 6 h. Then, 20 μL of the mixture was added to 180 μL of neutralization solution (PBS containing 5 g / L sodium thiosulfate and 0.5 g / L Tween 80) for 5 min to terminate the reaction. 50 μL of the sample solution was placed on a nutrient agar plate, spread evenly with a sterile L-stick, and incubated at 37℃ for 24 h. Colony counting was performed. The test was repeated three times, and the average kill rate (logarithmic sterilization value after action time) was calculated. The test results are shown in Table 3.

[0091] Table 3. Test results of bactericidal and antiviral properties of the antibacterial and antiviral agents in Example 3 and Comparative Examples 4-6.

[0092]

[0093] As can be seen from the data in the table, in conjunction with Examples 3 and Comparative Examples 4-6, and in conjunction with Tables 2 and 3, the antibacterial and antiviral agent prepared in this application has excellent long-lasting bactericidal performance. When no silica-loaded silver nanoparticles are added, the bactericidal rate is significantly reduced after 3 and 6 hours. The antibacterial and antiviral agent with only 20-50 nm silica-loaded silver nanoparticles added has a better bactericidal rate after 3 and 6 hours than the one without silica-loaded silver nanoparticles, but it is still significantly reduced. The addition of 100-300 nm silica-loaded silver nanoparticles can maintain the long-lasting antibacterial performance of the antibacterial and antiviral agent.

[0094] Test Example 3: Sterilization Test of Sanitary Wipes

[0095] In this test, Example 3 was used as an example. The antibacterial and antiviral agents prepared in Example 3 and Comparative Examples 4-6 were applied to sanitary wipes to obtain disinfectant wipes.

[0096] The specific method is as follows:

[0097] (1) At room temperature, mix 0.02% stabilizer (EDTA-2Na), 0.4% antibacterial and antiviral agent, and the remainder is purified water by mass percentage and stir for 15 minutes to obtain sanitary wipe liquid;

[0098] (2) Cut the pure cotton cloth into the required size according to the target specifications. Then, the wet wipe cloth and sanitary wet wipe liquid are mixed in a weight ratio of 1:5.6 by spraying or soaking to prepare the finished wet wipe. The water content of the wet wipe is controlled at 5.2 times, thus obtaining the disinfectant wet wipe.

[0099] 1) Sterilization performance test at room temperature

[0100] Disinfecting wipes prepared with antibacterial and antiviral agents according to GB15979-2002 "Hygienic Standard for Disposable Sanitary Products" were tested against Escherichia coli, Staphylococcus aureus, and Candida albicans. The experimental conditions were: using wipes as a carrier, bactericidal action time was 30 seconds and 1 minute, respectively. The experimental results are shown in Tables 4 and 5.

[0101] Table 4. Results of the bactericidal performance test of the sanitary wipes liquid in Example 3 and Comparative Examples 4-6 for 30 seconds.

[0102]

[0103] Table 5. Results of the bactericidal performance test of the sanitary wipes in Example 3 and Comparative Examples 4-6 after 1 minute.

[0104]

[0105] The data in the table shows that the disinfectant wipes provided by this invention have excellent bactericidal performance. Within 30 seconds, the bactericidal rate against *Escherichia coli* and *Staphylococcus aureus* is >99.9%, and the bactericidal rate against *Candida albicans* is >98.9%. At 1 minute, the bactericidal rate against *Escherichia coli* and *Staphylococcus aureus* reaches 100%, indicating that the disinfectant wipes have strong antibacterial effects and meet the requirements of GB15979-2024, the "Hygienic Requirements for Disposable Sanitary Products". Looking at the bactericidal rates of Example 3 and Comparative Examples 4-6, the bactericidal rate is relatively low when no silica-loaded silver nanoparticles are added, which may be related to the low content of active ingredients in the disinfectant wipes. Furthermore, the addition of 20-50 nm silica-loaded silver nanoparticles can effectively improve the bactericidal efficiency of the antibacterial and antiviral agent, achieving rapid sterilization. However, the addition of 100-300 nm silica-loaded silver nanoparticles has limited effect on improving the bactericidal rate.

[0106] Test Example 4: Security Performance Test

[0107] 1) Skin irritation performance test

[0108] Test method: The sanitary wipe liquid prepared with the antibacterial and antiviral agent provided in this application (taking Example 3 as an example, the same below) was tested according to the skin irritation test (multiple complete skin irritation tests): Appendix F (normative) of GB 15979-2024 "Hygienic Requirements for Disposable Sanitary Products"; WS / T 10009-2023 7.3 "Test Methods for Disinfection Products".

[0109] Evaluation basis: GB 15979-2024, "Hygienic Requirements for Disposable Sanitary Products"

[0110] Results: In the skin irritation test (multiple intact skin irritation tests) of the sanitary wipe liquid of this application, the local skin reaction irritation index of 3 Japanese white rabbits was 0.00 (0 - <0.5), and the skin irritation intensity was non-irritating. The results meet the relevant requirements in GB / 15979-2024 "Hygienic Requirements for Disposable Products".

[0111] The irritation index of the sanitary wipe liquid provided in this application is 0.00 when used in wipes, indicating that it is non-irritating. This demonstrates that the sanitary wipe liquid can be used to prepare mild, safe, and non-irritating disinfectant wipes.

[0112] 2) Acute eye irritation test

[0113] Test method: The sanitary wipe liquid prepared with the antibacterial and antiviral agent provided in this application (taking Example 3 as an example, the same below) was tested in accordance with Appendix F (normative) of GB 19797-2024 "Hygienic Requirements for Disposable Sanitary Products" and WS / T 10009-2024 7.4 "Test Methods for Disinfection Products".

[0114] Evaluation basis: GB 15979-2024, "Hygienic Requirements for Disposable Sanitary Products"

[0115] Results: The sanitary wipe liquid of this application was tested in acute eye irritation tests on Japanese white rabbits. The average scores of corneal damage, iris damage, conjunctival hyperemia, and conjunctival edema in three animals at three different observation time points (24h, 48h, and 72h) were 0 / 0 / 0 / 0; 0 / 0 / 0 / 0; and 0 / 0 / 0 / 0, respectively. The scores for corneal damage <1, iris damage <1, conjunctival hyperemia <2, and conjunctival edema <2, and the recovery time was <21 days. The eye irritation injury type was non-irritating, and the results met the relevant requirements in GB 15979-2024 "Hygienic Requirements for Disposable Sanitary Products".

[0116] In summary, the skin irritation test and acute eye irritation test show that the sanitary wipe liquid provided in this application can be used to prepare mild, safe, and non-irritating disinfectant wipes.

[0117] Test Example 5: Virus Inactivation Test

[0118] 1) Neutralizer identification test

[0119] Test sample: Antibacterial and antiviral agent prepared in Example 3

[0120] Test method: The neutralizing agent was RPMI 1640 + 3% sodium thiosulfate. The extruded liquid of the disinfectant wipes in this application was used and allowed to act for 30 minutes. The test results met the requirements of 2.1.1.10.5 of <<Disinfection Technical Specifications>> (2002 edition).

[0121] 2) Virus testing items:

[0122] a) Norovirus (MNV) inactivation test

[0123] Test method: According to Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition), virus inactivation test.

[0124] Preparation of virus suspension: Refer to section 2.1.1.10.3 of the "Disinfection Technical Specifications" (2002 edition) for the preparation of virus suspension;

[0125] Neutralizing agent identification test: Refer to the identification test of residual disinfectant chemical neutralization method in 2.1.1.10.5 of "Disinfection Technical Specifications" (2002 edition). The test sample used is the squeezed liquid of disinfectant wipes. The test was carried out for 30 minutes. The test temperature was controlled at (20±1)℃ in a water bath. The test was repeated 3 times.

[0126] Virus inactivation test: The test was conducted in accordance with the polio virus inactivation test 2.1.1.10.7 of the "Disinfection Technical Specifications" (2002 edition). The sample used in the test was the squeezed liquid of disinfectant wipes. The test was carried out for 30 minutes, and the water bath temperature was controlled at (20±1)℃. The test was repeated 3 times.

[0127] Evaluation basis: Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0128] Test results:

[0129] Norovirus (MNV) inactivation test: After three repeated tests, the test sample was the squeezed liquid of disinfectant wipes, and the action time was 30 minutes. The average log inactivation value of norovirus (MNV) was >4.00 and the inactivation rate was >99.99%, which met the requirements of 2.1.1.10 of the "Disinfection Technical Specification" (2002 edition).

[0130] b) Human papillomavirus (HPV16) inactivation test

[0131] Test method: According to Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition), virus inactivation test.

[0132] Evaluation basis: Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0133] Test results:

[0134] Human papillomavirus (HPV16) inactivation test: The test sample was the squeezed liquid of disinfectant wipes. After 30 minutes of contact, the log value of inactivation of human papillomavirus (HPV16) was >4.00, and the virus inactivation rate was >99.99%, which meets the requirements of 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0135] c) Hand-foot-mouth disease virus inactivation test

[0136] Test method: According to Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition), virus inactivation test.

[0137] Evaluation basis: Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0138] Test results:

[0139] Hand-foot-mouth disease virus inactivation test: The test sample was the squeezed liquid of disinfectant wipes. After 30 minutes of contact, the log value of inactivation of hand-foot-mouth disease virus was >4.00, and the virus inactivation rate was >99.99%, which meets the requirements of 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0140] d) Mycoplasma pneumoniae inactivation test

[0141] Test method: According to Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition), virus inactivation test.

[0142] Evaluation basis: Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0143] Test results:

[0144] Mycoplasma pneumoniae inactivation test: After three repeated tests, the test sample was the squeezed liquid of disinfectant wipes. After 30 minutes of action, the average log inactivation value of Mycoplasma pneumoniae was >5.00 and the inactivation rate was >99.99%, which meets the requirements of 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0145] e) Inactivation test of influenza A virus (H1N1)

[0146] Test method: According to Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition), virus inactivation test.

[0147] Evaluation basis: Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0148] Test Results: Inactivation Test of Influenza A Virus (H1N1): After three repeated tests, the test sample was the squeezed liquid of disinfectant wipes. After 30 minutes of contact, the average logarithmic inactivation value of influenza A virus (H1N1) (ATCC VR-1469) was >4.00, and the inactivation rate was >99.99%, which meets the requirements of 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0149] f) Human enterovirus 71 (EV-71) inactivation test

[0150] Test method: According to Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition), virus inactivation test.

[0151] Evaluation basis: Part II, Section 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0152] Test Results: Human Enterovirus 71 (EV-71) Inactivation Test: After three repeated tests, the test sample was the squeezed liquid of disinfectant wipes. After 30 minutes of contact, the average logarithmic inactivation value of human enterovirus 71 (EV-71) (ATCC VR-1432) was >4.00, and the inactivation rate was >99.99%, which meets the requirements of 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition).

[0153] In summary, the antibacterial and antiviral agent provided by this invention produces a sanitary wipe liquid with excellent antiviral properties, exhibiting excellent inactivation effects against various viruses such as influenza A virus (H1N1), human enterovirus 71 (EV-71), norovirus (MNV), human papillomavirus (HPV16), hand-foot-and-mouth disease virus, and mycoplasma pneumoniae.

[0154] Test Column 6: Wet Wipes Performance Test

[0155] In this test example, the disinfectant wipes prepared from the antibacterial and antiviral agent in Example 3 were tested according to the inductively coupled plasma mass spectrometry method in Chapter 4, Section 1.6 of the "Cosmetic Safety Technical Specifications" (2015 edition). The metal ion content in the sanitary wipe liquid (test sample was the extruded liquid of the disinfectant wipes) of this application was determined. The results were: lead < 0.03 mg / kg, arsenic < 0.001 mg / kg, mercury < 0.001 mg / kg, cadmium < 0.001 mg / kg, all of which comply with the relevant provisions in GB / T 27728.1-2024.

[0156] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention, and they should all be covered within the scope of the claims and specification of the present invention.

Claims

1. An antibacterial and antiviral agent, characterized in that, The product comprises the following components by weight: 100 parts water, 0.04-0.1 parts cetylpyridinium chloride, 0.2-0.6 parts benzalkonium chloride, 0.1-0.3 parts polyhexamethylene biguanide hydrochloride, 0.04-0.16 parts phenoxyethanol, 0.5-3 parts silica-supported silver nanoparticles, 0.4-1.0 parts propylene glycol, 0.02-0.06 parts glycerol, and 0.02-0.06 parts EDTA-2Na.

2. The antibacterial and antiviral agent according to claim 1, characterized in that, The silica-supported silver nanoparticles are a mixture of silica-supported silver nanoparticles with a particle size of 20-50 nm and silica-supported silver nanoparticles with a particle size of 100-300 nm, with a mass ratio of 1:(2-5).

3. The antibacterial and antiviral agent according to claim 1, characterized in that, The silica-supported silver nanoparticles were obtained by the following preparation method: 1) Disperse nano-silica microspheres in ethanol / water solution, adjust the pH of the reaction system to 4-5, and after ultrasonic dispersion, add γ-mercaptopropyltrimethoxysilane for grafting reaction, centrifuge and wash to obtain modified nano-silica microspheres. 2) Dissolve the modified nano-silica microspheres from step 1) in deionized water, then add silver nitrate solution, stir evenly, and then add L-ascorbic acid solution dropwise to carry out the reduction reaction. Centrifuge the reduction product to obtain the reaction product, wash and dry the reaction product to obtain silica-loaded silver nanoparticles.

4. The antibacterial and antiviral agent according to claim 1, characterized in that, The grafting reaction conditions described in step 1) are: reacting in a water bath at 60-80℃ for 4-8 hours.

5. The antibacterial and antiviral agent according to claim 1, characterized in that, The mass ratio of the nano-silica microspheres and γ-mercaptopropyltrimethoxysilane in step 1) is (5-15):(0.5-5).

6. The antibacterial and antiviral agent according to claim 1, characterized in that, In step 2), the modified nano-silica microspheres have a mass ratio of silver nitrate to L-ascorbic acid of (5-15):(0.3-1.0):(0.1-0.6).

7. The antibacterial and antiviral agent according to claim 1, characterized in that, The reduction reaction in step 2) is carried out at a pH of 7.0-8.0 and at 40-80°C for 1-3 hours.

8. A method for preparing an antibacterial and antiviral agent according to any one of claims 1-7, characterized in that, Includes the following steps: S1. Weigh an appropriate amount of purified water and add it to the mixing tank. Set the temperature to 50-60℃. Then add the weighed cetylpyridinium chloride, benzalkonium chloride, polyhexamethylene biguanide hydrochloride, and EDTA-2Na to the purified water in sequence to form a complex. Stir and disperse the mixture evenly at a speed of 50-150 rpm. Keep the temperature at 50-60℃ for 30-45 minutes. S2. Turn off the heating system, turn on the stirrer to cool naturally. When the temperature of the composite material drops below 40℃, slowly add phenoxyethanol, propylene glycol and glycerin in sequence. Stir evenly, then add silica-supported silver nanoparticles and continue stirring until evenly dispersed. Turn off the stirrer, take a sample for testing and discharge after it passes the test.

9. A disinfectant wipe, comprising a non-woven fabric substrate and a sanitary wipe liquid, characterized in that, The sanitary wipe liquid includes the antibacterial and antiviral agent as described in any one of claims 1-6.

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