An antibacterial wet wipe and a method of making

Abstract

This invention discloses an antibacterial wet wipe and its preparation method, comprising: a fiber substrate and an antibacterial wet wipe liquid; the fiber substrate is a spunlace nonwoven fabric treated with an amphiphilic chitosan derivative and a thermosensitive hydrogel; the antibacterial wet wipe liquid is composed of the following parts by weight: 1.8-2.5 parts of metal-organic framework antibacterial material, 85.5-90 parts of deionized water, 1.5-2.5 parts of glycerin, 2.5-3.5 parts of butylene glycol, 0.4-0.6 parts of ethylhexylglycerin, 0.25-0.35 parts of panthenol, 0.25-0.35 parts of PEG-40 hydrogenated castor oil, and 0 parts of citric acid. The antibacterial wipes contain 0.12-0.18 parts of sodium citrate, 0.20-0.30 parts of allantoin, 0.25-0.35 parts of sodium hyaluronate, and 0.08-0.12 parts of phenoxyethanol. The pH value of the antibacterial wipes is 5.5-6.0. The wipes are free of alcohol and quaternary ammonium salts, and are formulated with MOF materials, phenoxyethanol, and ethylhexylglycerin to avoid irritation. A weakly acidic environment of 5.5-6.0 is maintained through a citric acid and sodium citrate buffer system, which helps maintain the stability of the MOF materials and polyphenolic compounds.

Description

Technical Field

[0001] This invention relates to the field of hygiene products technology, and in particular to an antibacterial wet wipe and its preparation method. Background Technology

[0002] Wet wipes are a convenient and quick personal hygiene product widely used in daily life, infant care, and medical and health fields. With consumers' increasing demands for health and hygiene, the demand for wet wipes with antibacterial properties is growing.

[0003] In existing technologies, antibacterial wet wipes mainly achieve their antibacterial function by adding antibacterial agents to the wipe liquid. Common antibacterial agents include quaternary ammonium compounds such as benzalkonium chloride and cetylpyridinium chloride, which have rapid bactericidal effects, but long-term use may irritate the skin, and bacteria are prone to developing drug resistance; silver-based antibacterial agents such as nano silver and colloidal silver have broad-spectrum antibacterial properties, but silver ions are easily oxidized and discolored, have poor stability, and are expensive. For example, Chinese patent CN115569083B discloses a high-moisture-content antibacterial wet wipe and its preparation method, although it uses sodium hyaluronate grafted onto PET fibers. While improving antibacterial stability, the oxidation problem of silver-based antibacterial agents themselves remains unresolved. Plant extracts, such as extracts from honeysuckle, coptis, and scutellaria, are natural and mild, but their active ingredients are easily deactivated, resulting in poor storage stability and unstable antibacterial effects. For example, Chinese patent CN121154432A discloses an antibacterial sanitary wipe and its preparation method. Although there are improvements in sustained release, problems such as poor dispersibility and unstable pH in practical applications still exist. Alcohol-based products evaporate quickly and have good bactericidal effects, but they dry out easily and are highly irritating, making them unsuitable for infants and people with sensitive skin.

[0004] The main problems with existing technologies include: excessive irritation: most antibacterial wipes contain irritating ingredients such as alcohol and quaternary ammonium salts, which may cause skin allergies and dryness with long-term use, making them unsuitable for sensitive skin and infants; poor storage stability: natural antibacterial ingredients (such as plant extracts) are easily oxidized and deactivated, and silver-based antibacterial agents are easily oxidized and discolored, resulting in a decrease in the antibacterial effect of the product during storage; and short duration of action: a single antibacterial system is prone to bacterial resistance, and the antibacterial ingredients are released too quickly, making it difficult to maintain a long-lasting antibacterial effect.

[0005] Therefore, those skilled in the art urgently need to provide an antibacterial wet wipe and its preparation method that reduces irritation and enhances stability and timeliness. Summary of the Invention

[0006] The purpose of this invention is to provide an antibacterial wet wipe and its preparation method to solve the problems existing in the prior art.

[0007] An antibacterial wet wipe and its preparation method are disclosed, comprising: a fiber substrate and an antibacterial wet wipe liquid; the fiber substrate is a spunlace nonwoven fabric treated with an amphiphilic chitosan derivative and a thermosensitive hydrogel; the antibacterial wet wipe liquid is composed of the following parts by weight: 1.8-2.5 parts of metal-organic framework antibacterial material, 85.5-90 parts of deionized water, 1.5-2.5 parts of glycerin, 2.5-3.5 parts of butylene glycol, 0.4-0.6 parts of ethylhexylglycerin, 0.25-0.35 parts of panthenol, 0.25-0.35 parts of PEG-40 hydrogenated castor oil, 0.12-0.18 parts of citric acid, 0.20-0.30 parts of sodium citrate, 0.25-0.35 parts of allantoin, 0.08-0.12 parts of sodium hyaluronate, and 0.5-0.7 parts of phenoxyethanol; the pH value of the antibacterial wet wipe liquid is 5.5-6.0.

[0008] Preferably, the metal-organic framework antibacterial material is a polyphenol-copper metal-organic framework material, and at least one of ellagic acid-copper MOF, chlorogenic acid-copper MOF, and rhubarb polyphenol-copper MOF is selected.

[0009] Preferably, the ellagic acid-copper MOF is prepared by the following steps: 8-12 parts by weight of ellagic acid and 18-26 parts by weight of copper acetate are added to 300-500 parts by weight of deionized water, and then placed in a high-pressure reactor for heating at a temperature of 110-130°C for 12-18 hours. After centrifugation at 8000-10000 rpm for 8-12 minutes, the mixture is dried in an oven at 50-70°C for 8-12 hours. Finally, the mixture is washed with water and ethanol and then dried to obtain the ellagic acid-copper MOF.

[0010] Preferably, the amphiphilic chitosan derivative is N-octylchitosan, which is prepared as follows: chitosan is dissolved in acetic acid solution, octanal is added, and the mixture is reacted at 60-80°C for 4-6 hours. Then, it is reduced with sodium borohydride, and after reduction, the precipitate is precipitated, washed, and dried to obtain N-octylchitosan.

[0011] Preferably, the thermosensitive hydrogel is a poly(N-isopropylacrylamide)-based hydrogel, comprising N-isopropylacrylamide monomer, crosslinking agent and initiator, prepared by free radical polymerization reaction, and its low critical solution temperature (LCST) is 32-35°C.

[0012] Preferably, the fiber substrate is treated by the following steps: immersing the spunlace nonwoven fabric in a treatment solution containing 0.3-0.8 parts by weight of an amphiphilic chitosan derivative and 0.5-1.2 parts by weight of a thermosensitive hydrogel, ultrasonically treating it at 30-50°C for 20-30 minutes, then drying it at 60-65°C for 3-5 minutes, and finally drying it at 35-40°C for 30-35 hours.

[0013] Preferably, the mass ratio of the fiber substrate to the antibacterial wipe liquid is 1:2-4, and the antibacterial wipe liquid has an initial inhibition rate of ≥99% against Staphylococcus aureus and Escherichia coli, and the inhibition rate remains ≥92% after being stored at 30°C and 75% relative humidity for 180 days.

[0014] A method for preparing antibacterial wet wipes includes the following steps: S1: Preparation of metal-organic framework antibacterial materials; S2: Preparation of amphiphilic chitosan derivatives and thermosensitive hydrogels; S3: Fiber substrate treatment: The spunlace nonwoven fabric is immersed in a treatment solution containing amphiphilic chitosan derivatives and thermosensitive hydrogel, and then dried to obtain the treated fiber substrate. S4: Preparation of antibacterial wipe liquid: Disperse metal-organic framework antibacterial materials in deionized water, add glycerin, butylene glycol, ethylhexylglycerin, panthenol, PEG-40 hydrogenated castor oil, citric acid, sodium citrate, allantoin, sodium hyaluronate and phenoxyethanol, then stir evenly and adjust the pH value to 5.5-6.0 to obtain antibacterial wipe liquid; S5: Apply the antibacterial wet wipe liquid at a temperature of 40-45℃ evenly to the treated fiber substrate by spraying, with a spraying amount of 120-180g / m². Then let it stand at 30-35℃ for 20-30 minutes to absorb the liquid. Finally, seal and package the product to obtain antibacterial wet wipes.

[0015] Compared with the prior art, the present invention provides an antibacterial wet wipe and its preparation method, which has the following beneficial effects: 1. Gentle and non-irritating: The antibacterial wipe liquid of this application is free of alcohol and quaternary ammonium salt irritating antibacterial agents. It uses MOF material combined with phenoxyethanol and ethylhexylglycerin to provide broad-spectrum antibacterial properties while avoiding the irritation of traditional antibacterial agents. At the same time, it is combined with multiple moisturizing and repairing ingredients, which have good skin compatibility and are suitable for sensitive skin and infants.

[0016] 2. Good storage stability: This invention maintains a weakly acidic environment with a pH value of 5.5-6.0 through a citric acid and sodium citrate buffer system, which is beneficial to maintaining the stability of MOF materials and polyphenolic compounds; the amphiphilic chitosan derivative and thermosensitive hydrogel composite treatment of the fiber substrate form a protective layer, which further improves the stability of antibacterial components.

[0017] 3. Increased timeliness: This application uses metal-organic framework (MOF) material as an antibacterial carrier. By utilizing the porous structure of MOF and the antibacterial properties of metal ions, the antibacterial components are released in a sustained manner. MOF material is formed by compounding with natural polyphenols, which can utilize the bioactivity of polyphenols and protect the active ingredients through the skeleton structure of MOF, thereby improving stability. Detailed Implementation

[0018] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0019] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the present invention will be further described in detail below with reference to specific embodiments.

[0020] An antibacterial wet wipe includes: a fiber substrate and an antibacterial wet wipe liquid; the fiber substrate is a spunlace nonwoven fabric that has been treated with an amphiphilic chitosan derivative and a thermosensitive hydrogel. The antibacterial wipe liquid is composed of the following parts by weight: 1.8-2.5 parts of metal-organic framework antibacterial material, 85.5-90 parts of deionized water, 1.5-2.5 parts of glycerin, 2.5-3.5 parts of butylene glycol, 0.4-0.6 parts of ethylhexylglycerin, 0.25-0.35 parts of panthenol, 0.25-0.35 parts of PEG-40 hydrogenated castor oil, 0.12-0.18 parts of citric acid, 0.20-0.30 parts of sodium citrate, 0.25-0.35 parts of allantoin, 0.08-0.12 parts of sodium hyaluronate, and 0.5-0.7 parts of phenoxyethanol; the pH value of the antibacterial wipe liquid is 5.5-6.0.

[0021] The antibacterial materials of the metal-organic framework are polyphenol-copper metal-organic framework materials, and at least one of ellagic acid-copper MOF, chlorogenic acid-copper MOF and rhubarb polyphenol-copper MOF is selected.

[0022] A method for preparing antibacterial wet wipes includes the following steps: S1: Preparation of metal-organic framework antibacterial materials: 8-12 parts by weight of ellagic acid and 18-26 parts by weight of copper acetate were added to 300-500 parts by weight of deionized water, and then placed in a high-pressure reactor for heating at 110-130℃ for 12-18 hours. After centrifugation at 8000-10000 rpm for 8-12 minutes, the mixture was dried in an oven at 50-70℃ for 8-12 hours. Finally, the mixture was washed with water and ethanol and dried to obtain ellagic acid-copper MOF. S2: Preparation of amphiphilic chitosan derivatives and thermosensitive hydrogels; The amphiphilic chitosan derivative is N-octylchitosan, which is prepared as follows: chitosan is dissolved in acetic acid solution, octanal is added, and the mixture is reacted at 60-80℃ for 4-6 hours. Then, it is reduced with sodium borohydride. After reduction, the precipitate is precipitated, washed, and dried to obtain N-octylchitosan. The thermosensitive hydrogel is a poly(N-isopropylacrylamide) (PNIPAM) based hydrogel, which contains N-isopropylacrylamide monomer, crosslinking agent and initiator, and is prepared by free radical polymerization reaction. Its low critical solution temperature (LCST) is 32-35℃. S3: Fiber substrate treatment: The spunlace nonwoven fabric is immersed in the treatment solution prepared in S2, which contains 0.3-0.8 parts by weight of amphiphilic chitosan derivative and 0.5-1.2 parts by weight of thermosensitive hydrogel. The solution is ultrasonically treated at 30-50℃ for 20-30 minutes, then dried at 60-65℃ for 3-5 minutes, and finally dried at 35-40℃ for 30-35 hours to obtain the treated fiber substrate. S4: Preparation of antibacterial wipe liquid: Disperse metal-organic framework antibacterial materials in deionized water, add glycerin, butylene glycol, ethylhexylglycerin, panthenol, PEG-40 hydrogenated castor oil, citric acid, sodium citrate, allantoin, sodium hyaluronate and phenoxyethanol, then stir evenly and adjust the pH value to 5.5-6.0 to obtain antibacterial wipe liquid; The mass ratio of the treated fiber substrate to the antibacterial wipe liquid is 1:2-4; S5: Apply the antibacterial wet wipe liquid at a temperature of 40-45℃ evenly to the treated fiber substrate by spraying, with a spraying amount of 120-180g / m². Then let it stand at 30-35℃ for 20-30 minutes to absorb the liquid. Finally, seal and package the product to obtain antibacterial wet wipes. Example

[0023] S1, Preparation of ellagic acid-copper MOF: 10g ellagic acid and 22g copper acetate were added to 400ml deionized water, transferred to a high-pressure reactor, heated to 120℃ and kept for 15 hours, then centrifuged at 9000rpm for 10 minutes, placed in a 60℃ oven and dried for 10 hours, washed with water and ethanol and then dried to obtain ellagic acid-copper MOF; S2, to prepare amphiphilic chitosan derivatives (N-octylchitosan) and thermosensitive hydrogels (poly-N-isopropylacrylamide (PNIPAM) based hydrogels). Preparation of N-octylchitosan: Dissolve 5g of chitosan in 200ml of 2% acetic acid solution, add 3g of octanal, react at 70℃ for 5 hours, then reduce with 2g of sodium borohydride, precipitate, wash, and dry to obtain N-octylchitosan. Preparation of poly(N-isopropylacrylamide) (PNIPAM) based hydrogel: 10g of N-isopropylacrylamide monomer, 0.2g of N,N'-methylenebisacrylamide crosslinking agent and 0.1g of ammonium persulfate initiator were dissolved in 100ml of deionized water and reacted at 60℃ for 6 hours under nitrogen protection to obtain PNIPAM hydrogel with LCST of 33℃; S3, fiber substrate treatment: Add 0.5g N-octyl chitosan and 0.8g PNIPAM hydrogel to 200ml deionized water and stir evenly to obtain a treatment solution. Immerse the spunlace nonwoven fabric in the treatment solution, sonicate it at 40℃ for 25 minutes, dry it at 62℃ for 4 minutes, and then dry it at 38℃ for 32 hours to obtain the treated fiber substrate. S4, Preparation of antibacterial wipe liquid: Disperse 2g ellagic acid-copper MOF in 88g deionized water, add 2g glycerin, 3g butylene glycol, 0.5g ethylhexylglycerin, 0.3g panthenol, 0.3g PEG-40 hydrogenated castor oil, 0.15g citric acid, 0.25g sodium citrate, 0.3g allantoin, 0.1g sodium hyaluronate, and 0.6g phenoxyethanol, stir evenly, and adjust the pH value to 5.8 to obtain antibacterial wipe liquid; S5. Apply antibacterial wet wipe liquid at 42℃ evenly to the treated fiber substrate by spraying at a rate of 150g / m². Then, let it stand at 32℃ for 25 minutes to absorb the liquid, seal and package it to obtain antibacterial wet wipes. Example

[0024] The method is basically the same as in Example 1, except that: chlorogenic acid-copper MOF is used instead of ellagic acid-copper MOF, and the amount used is 2.2g; the amount of glycerin in the antibacterial wipe liquid is 2.3g, and the amount of butylene glycol is 3.5g. Example

[0025] The method is basically the same as in Example 1, except that rhubarb polyphenol-copper MOF is used instead of ellagic acid-copper MOF, and the dosage is 1.8g; the dosage of phenoxyethanol in the antibacterial wipe liquid is 0.5g.

[0026] Comparative Example 1: The example is basically the same as Example 1, except that: nano-silver is used instead of ellagic acid-copper MOF, and the amount is 2g; and no thermosensitive hydrogel is added.

[0027] Comparative Example 2: Basically the same as Example 1, except that: benzalkonium chloride was used instead of ellagic acid-copper MOF, and the amount was 2g; no amphiphilic chitosan derivative was added.

[0028] Antibacterial performance test: The antibacterial properties of the antibacterial wet wipes prepared in Examples 1-3 and Comparative Examples 1-2 were tested, and the results are shown in Table 1 (storage conditions: 30°C and 75% relative humidity):

[0029] Skin irritation test: Skin irritation tests were conducted on the antibacterial wet wipes prepared in Examples 1-3 and Comparative Examples 1-2. The results are shown in Table 2.

[0030] Moisturizing test: Moisturizing tests were conducted on the antibacterial wet wipes prepared in Examples 1-3 and Comparative Examples 1-2. The results are shown in Table 3.

[0031] Test results show that the antibacterial wet wipes of the present invention have good antibacterial properties, long-lasting stability and skin compatibility, and their overall performance is significantly better than that of the comparative example.

[0032] The embodiments described above are merely preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Various modifications and improvements made by those skilled in the art to the technical solutions of the present invention without departing from the spirit of the present invention should fall within the protection scope defined by the claims of the present invention.

Claims

1. An antibacterial wet wipe, characterized by, include: Fiber base and antibacterial wipe liquid; The fiber substrate is a spunlace nonwoven fabric that has undergone composite treatment with amphiphilic chitosan derivatives and thermosensitive hydrogel; The antibacterial wipe liquid is composed of the following parts by weight: 1.8-2.5 parts of metal-organic framework antibacterial material, 85.5-90 parts of deionized water, 1.5-2.5 parts of glycerin, 2.5-3.5 parts of butylene glycol, 0.4-0.6 parts of ethylhexylglycerin, 0.25-0.35 parts of panthenol, 0.25-0.35 parts of PEG-40 hydrogenated castor oil, 0.12-0.18 parts of citric acid, 0.20-0.30 parts of sodium citrate, 0.25-0.35 parts of allantoin, 0.08-0.12 parts of sodium hyaluronate, and 0.5-0.7 parts of phenoxyethanol; the pH value of the antibacterial wipe liquid is 5.5-6.

0.

2. The antibacterial wet wipe according to claim 1, characterized in that, The metal-organic framework antibacterial material is a polyphenol-copper metal-organic framework material, and at least one of ellagic acid-copper MOF, chlorogenic acid-copper MOF, and rhubarb polyphenol-copper MOF is selected.

3. The antibacterial wet wipe according to claim 2, characterized in that, The ellagic acid-copper MOF is prepared by the following steps: 8-12 parts by weight of ellagic acid and 18-26 parts by weight of copper acetate are added to 300-500 parts by weight of deionized water, and then placed in a high-pressure reactor for heating at 110-130°C for 12-18 hours. After centrifugation at 8000-10000 rpm for 8-12 minutes, the mixture is dried in an oven at 50-70°C for 8-12 hours. Finally, the mixture is washed with water and ethanol and then dried to obtain the ellagic acid-copper MOF.

4. The antibacterial wet wipe according to claim 1, characterized in that, The amphiphilic chitosan derivative is N-octylchitosan, and its preparation method is as follows: chitosan is dissolved in acetic acid solution, octanal is added, and the reaction is carried out at 60-80℃ for 4-6 hours. Then, it is reduced with sodium borohydride. After reduction, the precipitate is precipitated, washed, and dried to obtain N-octylchitosan.

5. The antibacterial wet wipe according to claim 1, characterized in that, The thermosensitive hydrogel is a poly(N-isopropylacrylamide) (PNIPAM) based hydrogel, which contains N-isopropylacrylamide monomer, crosslinking agent and initiator, and is prepared by free radical polymerization reaction. Its low critical solution temperature (LCST) is 32-35℃.

6. The antibacterial wet wipe according to claim 1, characterized in that, The fiber substrate is treated by the following steps: the spunlace nonwoven fabric is impregnated in a treatment solution containing 0.3-0.8 parts by weight of amphiphilic chitosan derivative and 0.5-1.2 parts by weight of thermosensitive hydrogel, ultrasonically treated at 30-50°C for 20-30 minutes, then dried at 60-65°C for 3-5 minutes, and finally dried at 35-40°C for 30-35 hours.

7. The antibacterial wet wipe according to claim 1, characterized in that, The mass ratio of the fiber substrate to the antibacterial wipe liquid is 1:2-4. The antibacterial wipe liquid has an initial inhibition rate of ≥99% against Staphylococcus aureus and Escherichia coli. After being stored at 30°C and 75% relative humidity for 180 days, the inhibition rate remains ≥92%.

8. The method for preparing an antibacterial wet wipe according to claims 1-7, characterized in that, Includes the following steps: S1: Preparation of metal-organic framework antibacterial materials; S2: Preparation of amphiphilic chitosan derivatives and thermosensitive hydrogels; S3: Fiber substrate treatment: The spunlace nonwoven fabric is immersed in a treatment solution containing amphiphilic chitosan derivatives and thermosensitive hydrogel, and then dried to obtain the treated fiber substrate. S4: Preparation of antibacterial wipe liquid: Disperse metal-organic framework antibacterial materials in deionized water, add glycerin, butylene glycol, ethylhexylglycerin, panthenol, PEG-40 hydrogenated castor oil, citric acid, sodium citrate, allantoin, sodium hyaluronate and phenoxyethanol, then stir evenly and adjust the pH value to 5.5-6.0 to obtain antibacterial wipe liquid; S5: Apply the antibacterial wet wipe liquid at a temperature of 40-45℃ evenly to the treated fiber substrate by spraying, with a spraying amount of 120-180g / m². Then let it stand at 30-35℃ for 20-30 minutes to absorb the liquid. Finally, seal and package the product to obtain antibacterial wet wipes.

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