A mild, non-irritating and odorless preservative and bactericidal agent, preparation method thereof, and daily chemical product

By using a compounded mild non-irritating antiseptic bactericide in wet wipes, the problems of irritability, high odor and weak antiseptic strength of existing wet wipes are solved, and the antiseptic, sterilization and soothing effects in wet wipes are improved, and the shelf life is extended.

CN119547795BActive Publication Date: 2025-04-29GUANGDONG DIMEI NEW MATERIAL TECH CO LTD
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Patent Information

Application Number
CN202510119744.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-01-25
Publication Date
2025-04-29
Estimated Expiration
2045-01-25

AI Technical Summary

Technical Problem

The existing wet wipes preservatives have poor experience in the wet wipes system due to their irritability, high odor, and weak anti-corrosion. The wet wipes are easily contaminated by microbial contamination, resulting in problems such as excessive bacterial colonies in the product, mildew spots, and yellowing.

Method used

A gentle, non-irritating and odorless antiseptic bactericide is used. This agent is compounded with antiseptic active ingredients, plant extracts (such as jujube extract and mulberry leaf extract), butanediol and water. By forming a solubilization system and synergistically, it ensures that the antiseptic active ingredients are evenly distributed in the wet wipes liquid and wet wipes, enhancing the sterilization, antiseptic and soothing effects.

Benefits of technology

It realizes the uniform distribution of anticorrosion and bactericide in wet wipes, enhances the anticorrosion and bactericidal effect of wet wipes, extends the shelf life of wet wipes, and has the characteristics of gentle, non-irritating and odorlessness. It is suitable for daily chemical products such as wet wipes.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to the technical field of daily chemical products, discloses a method for preparing a mild, non-irritating and odorless antiseptic and bactericidal agent, provides an antiseptic and bactericidal active ingredient and a plant extract, mixes the antiseptic and bactericidal active ingredient, the plant extract, butylene glycol and water, and after complete dissolution, obtains a mild, non-irritating and odorless antiseptic and bactericidal agent; wherein the antiseptic and bactericidal active ingredient is composed of lauroyl arginine ethyl ester hydrochloride, benzalkonium chloride, cetylpyridinium chloride, polyaminopropyl biguanide and benzoic acid, and the plant extract is composed of jujube extract and mulberry leaf extract. The present invention can synergize after compounding the antiseptic and bactericidal active ingredient, water, butylene glycol and plant extract, enhance the bactericidal, antiseptic and soothing effects of the antiseptic and bactericidal active ingredient in wet wipes, and improve its stability in the wet wipes system, and prevent the situation that the antiseptic and bactericidal active ingredient is unevenly distributed in the wet wipes liquid and the wet wipes cloth, resulting in insufficient antiseptic strength and microbial contamination.
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Description

Technical Field

[0001] The invention belongs to the technical field of daily chemical products, and specifically relates to a mild, non-irritating and odorless preservative and bactericidal agent, a preparation method thereof, and a daily chemical product. Background Art

[0002] At present, there are few preservatives and fungicides specifically for wet wipes on the market. Most wet wipes manufacturers choose traditional preservatives such as: Kasson is highly irritating and is prohibited from being used in leave-on products; formaldehyde releasers are harmful to the human body; parabens may affect the endocrine system and cause skin allergies; chlorphenesin has weak preservative ability and a strong odor; phenoxyethanol has weak preservative power and a large amount of addition can cause fever and allergies; benzalkonium chloride will be absorbed by the cloth, and the preservative active ingredients in the liquid are reduced or basically eliminated, leading to microbial risks. There are also other "no added preservatives" in cosmetics such as glyceryl caprylate, ethylhexylglycerin, caprylyl glycol, 1,2-hexanediol, etc., which also have a strong odor and weak preservative power. Overall, these preservatives have a poor experience in the wet wipes system due to various problems. Those who have been involved in this industry know that wet wipes are more susceptible to microbial contamination than personal care products, and it is difficult to prevent wet wipes from corrosion and mildew. Although wet wipes contain preservatives such as those mentioned above, the special nature of wet wipe materials has caused many wet wipe companies to have problems caused by a series of microbial contamination, such as excessive total bacterial colony counts, mold spots, yellowing, etc. Moreover, wet wipes products cannot be recalled and reprocessed like other products, which causes significant losses to the companies and also affects the health of uninformed consumers.

[0003] The main reason for the difficulty in preserving wet wipes lies in the material properties of the wet wipes themselves, whether it is a non-woven fabric made of fibers such as polyester, polypropylene, polyamide, and viscose, or a cotton cloth made of 100% pure cotton. These fabrics are very conducive to the attachment and growth of microorganisms due to their own porous structure, and the polysaccharide structure of the fibers is similar to the extracellular polysaccharides of bacteria, which is conducive to the formation of biofilms and provides more nutrients for the growth and reproduction of microorganisms; in addition, these porous structures and the electrostatic adsorption capabilities of the fibers make some preservatives adsorbed in the fibers, resulting in the water phase not being protected by a sufficient concentration of preservatives. Therefore, the raw materials of wet wipes are likely to be full of microorganisms before production. At the same time, if microbial contamination is introduced during the production process, it will also make it difficult to kill the microorganisms. These will bring huge invisible risks to the production of wet wipes.

[0004] On the other hand, there is no internationally accepted method for the antiseptic challenge of wet wipes. Therefore, when dealing with the antiseptic challenge of wet wipes, most testing agencies test the extruded liquid of wet wipes according to the liquid antiseptic challenge method commonly used in cosmetics. This will cause two situations: ① For some traditional preservatives that are not easily adsorbed on the fibers of wet wipes, because the antiseptic system is basically in the wet wipe liquid and there is no preservative in the wet wipe cloth, the wet wipe liquid can achieve very good antiseptic challenge results; ② For wet wipe products that will be adsorbed by the wet wipe cloth, there is basically no preservative residue in the wet wipe liquid, which will lead to terrible challenge results. However, wet wipes are mainly composed of wet wipe liquid and wet wipe cloth. Both the wet wipe liquid and the wet wipe cloth are very easy to be contaminated by microorganisms. Therefore, wet wipe products occasionally have microbial problems during actual production and storage, proving that the antiseptic challenge results made by using only wet wipe liquid cannot fully and truly reflect the antiseptic efficacy of wet wipe products, resulting in the fact that the wet wipe preparation companies rely on experimental results to evaluate the microbial risks in actual production. This method has little reference significance. Summary of the invention

[0005] In view of this, one of the objects of the present invention is to provide a mild, non-irritating and odorless preservative and bactericidal agent and a preparation method thereof. By combining the preservative and bactericidal active ingredients with the plant extracts, when the preservative and bactericidal agent is applied to daily chemical products such as wet wipes, on the one hand, the adsorption amount of the preservative and bactericidal active ingredients by the wet wipes can be fixed, so that both the wet wipes and the wet wipes liquid have sufficient preservative and bactericidal active ingredients to resist microbial contamination. On the other hand, the wet wipes prepared with the preservative and bactericidal agent also have a certain effect on removing acne, and are mild, non-irritating and odorless, and have a certain soothing effect.

[0006] The second object of the present invention is to provide a daily chemical product, by adding a small amount of antiseptic and bactericidal agent to the daily chemical product, the daily chemical product such as wet wipes can achieve good antiseptic, bactericidal, acne-removing and soothing effects. The antiseptic and bactericidal agent of the present invention can effectively extend the shelf life of the wet wipes, ensure the safety during use and be good to the skin.

[0007] To achieve the purpose of the present invention, the technical solution adopted by the present invention is:

[0008] A method for preparing a mild, non-irritating and odorless antiseptic and fungicide, comprising providing an antiseptic and fungicide active ingredient and a plant extract, mixing the antiseptic and fungicide active ingredient, the plant extract, butanediol and water, and preparing the mild, non-irritating and odorless antiseptic and fungicide after the mixture is completely dissolved;

[0009] The antiseptic and bactericidal active ingredients are composed of lauroyl arginine ethyl ester hydrochloride, benzalkonium chloride, cetylpyridinium chloride, polyaminopropyl biguanide and benzoic acid, and the plant extracts are composed of jujube extract and mulberry leaf extract.

[0010] In the present invention, jujube and mulberry leaf contain a variety of natural active ingredients, which can destroy the structure of pathogen membranes, kill or inhibit certain pathogens, and have a good conditioning effect on the skin, improve and regulate the metabolism of skin tissue, and have soothing effects. Specifically, jujube is a deciduous tree of the Rhamnaceae family, and its extract contains relatively rich sugars, amino acids, vitamins, flavonoids, polyphenols, saponins, alkaloids and other ingredients, which have antioxidant, alcohol-relieving, anti-aging, antibacterial and anti-inflammatory effects, and are often made into health-care foods. The main active ingredients of mulberry leaf extract are mainly isopentenyl flavonoid compounds, and in addition, they also contain alkaloids, organic acids, coumarins, triterpenoid compounds, etc. These ingredients have excellent antioxidant, soothing and anti-inflammatory, insecticidal, anti-pathogenic microorganism, hypoglycemic effects, etc.

[0011] The present invention can synergistically enhance the efficacy of two plant extracts, water, butylene glycol, lauroyl arginine ethyl ester hydrochloride, benzalkonium chloride, cetylpyridinium chloride, polyaminopropyl biguanide and benzoic acid after compounding, thereby enhancing the bactericidal, antiseptic and soothing effects of the antiseptic and bactericidal active ingredients in the wet wipes, and improving the stability thereof in the wet wipes system (the content of the antiseptic and bactericidal active ingredients in the wet wipes cloth and the wet wipes liquid), thereby preventing the occurrence of microbial contamination due to the uneven distribution of the antiseptic and bactericidal active ingredients in the wet wipes liquid and the wet wipes cloth, resulting in insufficient antiseptic strength.

[0012] The present invention uses a mixed solution of water and butanediol as a solvent system, and the purpose is to make the added antiseptic and bactericidal active ingredients fully dissolve and stably exist in the solution, without precipitation precipitation or the solution becoming viscous paste and other phenomena, the lauroyl arginine ethyl ester hydrochloride, benzalkonium chloride, cetylpyridinium chloride, polyaminopropyl biguanide added in the solvent have a certain surface activity in addition to antiseptic and bactericidal effects, and can form a solubilization system, so that the added jujube extract, mulberry leaf extract, benzoic acid are completely dissolved, and the antiseptic and bactericidal agent prepared in this way can be completely dissolved in water without precipitation. In addition, benzoic acid can significantly improve the adsorption of lauroyl arginine ethyl ester hydrochloride, benzalkonium chloride, cetylpyridinium chloride, polyaminopropyl biguanide in cloth, and two plant extracts can also enhance the mildness of the antiseptic and bactericidal active ingredients and reduce their irritation. The stability and usability of the antiseptic and bactericidal agent and its wet wipes product are guaranteed, and the service life of the wet wipes product is effectively extended.

[0013] The preparation method of the mild, non-irritating and odorless antiseptic and bactericidal agent of the present invention is simple to operate, low in cost and easy to industrialize and produce.

[0014] Furthermore, the preparation method of the mild, non-irritating and odorless antiseptic bactericidal agent of the present invention comprises the following steps:

[0015] S10, preparing jujube extract and mulberry leaf extract;

[0016] S20, mixing water and butanediol uniformly to obtain a mixed solution, and then adding benzalkonium chloride, polyaminopropyl biguanide, lauroyl arginine ethyl ester hydrochloride, benzoic acid, and cetylpyridinium chloride to the mixed solution in sequence, heating and stirring to obtain a colorless transparent solution;

[0017] S30, adding the jujube extract and the mulberry leaf extract into the colorless transparent solution, stirring evenly, to prepare a mild, non-irritating and odorless preservative and bactericidal agent.

[0018] Furthermore, the mass ratio of benzalkonium chloride, polyaminopropyl biguanide, lauroyl arginine ethyl ester hydrochloride, cetylpyridinium chloride, benzoic acid, jujube extract, mulberry leaf extract, water and butylene glycol is (1-20): (1-20): (0.5-10): (1-20): (1-20): (1-8): (1-5): (10-25): (20-35). For example: 15:15:3:10:8:4:3:18:24, 10:10:7:10:10:4:3:15:31, 12:12:5:12:12:5:2:20:20 or 8:8:3:15:11:4:1:20:30, etc., which are not listed one by one. By optimizing the ratio of each component of the antiseptic and bactericidal active ingredient, the bactericidal, antiseptic and soothing effects of the antiseptic and bactericidal active ingredient in the wet wipes can be enhanced, and its stability in the wet wipes system (the content of the antiseptic and bactericidal active ingredient in the wet wipes cloth and wet wipes liquid) can be improved to prevent the uneven distribution of the antiseptic and bactericidal active ingredients in the wet wipes liquid and cloth, resulting in insufficient antiseptic strength and microbial contamination. When the water content is too much and the alcohol content is too low, it will affect the product stability of the antiseptic and bactericidal agent itself, such as turning into a viscous paste-like semi-solid state; anyway, if the alcohol content is high and the water content is low, active ingredients will precipitate crystals.

[0019] Further, step S10 is specifically as follows: crushing the jujube and mulberry leaves respectively, then adding a 50% (volume fraction) ethanol solution at a material-liquid mass ratio of 1: (15-20), respectively performing ultrasonic extraction, filtering after ultrasonic extraction, collecting the filtrate, repeating the above operation twice, combining the filtrate, evaporating and concentrating the filtrate under reduced pressure, and vacuum drying to obtain the jujube extract and the mulberry leaf extract. Among them, reduced pressure evaporation concentration and vacuum drying are both conventional techniques in the art, and will not be described in detail.

[0020] Further, the heating temperature in step S20 is 40°C~60°C. Among them, cetylpyridinium chloride is very easy to agglomerate when encountering liquid during the mixing and stirring process, and it is difficult to dissolve. When its investment is too high, it will affect the production timeliness and increase the production cost, and the antiseptic and bactericidal properties of the remaining raw materials are not much different from those of cetylpyridinium chloride, and are more soluble. Benzoic acid, jujube extract, and mulberry leaf extract have poor solubility in water and alcohol mixed solvents. Adding benzalkonium chloride, lauroyl arginine ethyl ester hydrochloride, cetylpyridinium chloride, and polyaminopropyl biguanide can improve the solubility of these three raw materials, and can also improve the stability of the antiseptic and bactericidal active ingredients themselves and added to other products. The temperature is selected between 40-60°C, which can improve the dissolution rate of the raw materials in the mixed solvent to avoid excessive water volatilization or long stirring time.

[0021] Furthermore, the heating and stirring time in step S20 is 2 h to 4 h.

[0022] On the other hand, a mild, non-irritating and odorless preservative and bactericidal agent is provided, which is prepared according to the preparation method of the mild, non-irritating and odorless preservative and bactericidal agent.

[0023] Furthermore, the mild, non-irritating and odorless preservative and bactericidal agent is prepared from the following raw materials by weight:

[0024] Benzalkonium chloride 1-20 parts;

[0025] 1-20 parts of polyaminopropyl biguanide;

[0026] 0.5-10 parts of lauroyl arginine ethyl ester hydrochloride;

[0027] 1-20 parts of cetylpyridinium chloride;

[0028] 1-20 parts of benzoic acid;

[0029] 1-8 parts of Ziziphus jujuba extract;

[0030] 1-5 parts of mulberry leaf extract;

[0031] 10~25 parts water;

[0032] 20-35 parts of butanediol.

[0033] The present invention optimizes the material ratio of each raw material to stabilize the system of the antiseptic and bactericidal agent. When added to the wet wipes product, the distribution of each component in the wet wipes liquid and the wet wipes cloth can be effectively controlled. The antiseptic and bactericidal agent has high antiseptic and bactericidal effects, and is mild, non-irritating and odorless. The antiseptic and bactericidal agent is a light yellow transparent liquid. The antiseptic and bactericidal agent of the present invention is mild, non-irritating and odorless, and has stable antiseptic and bactericidal effects.

[0034] On the other hand, a daily chemical product is provided, comprising a preservative and bactericide, wherein the preservative and bactericide is prepared by using the mild, non-irritating and odorless preservative and bactericide.

[0035] Furthermore, the daily chemical product is wet wipes liquid or wet wipes containing the wet wipes liquid.

[0036] Furthermore, the mild, non-irritating and odorless preservative and bactericidal agent is added to the wet wipes liquid in an amount of 0.4%-0.6%, preferably 0.5%.

[0037] Beneficial effects of the present invention:

[0038] The present invention can synergistically enhance the efficacy of several antiseptic and bactericidal active ingredients, water, butylene glycol and plant extracts after compounding, enhance the bactericidal, antiseptic and soothing effects of the antiseptic and bactericidal active ingredients in wet wipes, and improve its stability in the wet wipe system (the content of the antiseptic and bactericidal active ingredients in the wet wipe cloth and wet wipe liquid), and prevent the occurrence of microbial contamination due to the uneven distribution of the antiseptic and bactericidal active ingredients in the wet wipe liquid and cloth, resulting in insufficient antiseptic strength. The antiseptic and bactericidal agent can be used in various wet wipe systems, and has the characteristics of good stability, low dosage, mildness, no irritation, and no odor in the wet wipe system. DETAILED DESCRIPTION

[0039] In order to enable those skilled in the art to better understand the technical solution of the present invention, the specific implementation methods are described in detail below. It should be understood that the following examples are only exemplary descriptions and explanations of the present invention, and should not be construed as limiting the scope of protection of the present invention. All technologies implemented based on the above content of the present invention are included in the scope that the present invention is intended to protect.

[0040] Example 1

[0041] The raw material ratio of the mild, non-irritating and odorless antiseptic and bactericidal agent of this embodiment is as shown in Table 1, and the specific preparation method is as follows:

[0042] S10, crushing the jujube and mulberry leaves respectively, then adding a 50% ethanol solution at a material-liquid mass ratio of 1:16, performing ultrasonic extraction respectively, filtering after ultrasonication, collecting the filtrate, repeating the above operation twice, combining the filtrate, evaporating and concentrating the filtrate under reduced pressure, and vacuum drying to obtain the jujube extract and the mulberry leaf extract;

[0043] S20. Mix water and butanediol evenly, then add benzalkonium chloride, polyaminopropyl biguanide, lauroyl arginine ethyl ester hydrochloride, benzoic acid and cetylpyridinium chloride to the above mixture in sequence, heat to 50°C and continue stirring for 2 h. After the previous material component is completely dissolved, add the next raw material, and stir until a colorless, transparent, uniform solution is obtained to obtain Liquid A.

[0044] S30, adding the jujube extract and mulberry leaf extract to the above liquid A and stirring until it becomes a light yellow transparent liquid to obtain a mild, non-irritating and odorless preservative and bactericidal agent.

[0045] Table 1 Raw material composition of Examples 1-12 and Comparative Examples 1-14 (unit: wt.%)

[0046]

[0047] The preparation methods of Examples 2-12 and Comparative Examples 1-14 are substantially the same as those of Example 1 above, and the proportions of the raw materials are shown in Table 1.

[0048] Comparative Example 15

[0049] This comparative example is substantially the same as Example 1, except that benzoic acid is not added and citric acid is used in an equal mass ratio.

[0050] Comparative Example 16

[0051] This comparative example is basically the same as Example 1, except that the jujube extract is not added and is replaced with an aloe extract of an equal weight ratio.

[0052] Comparative Example 17

[0053] This comparative example is basically the same as Example 1, except that the jujube extract is not added and is replaced with chamomile extract in an equal mass ratio.

[0054] Comparative Example 18

[0055] This comparative example is basically the same as Example 1, except that the jujube extract is not added and is replaced with a tea tree extract of an equal mass ratio.

[0056] Comparative Example 19

[0057] This comparative example is basically the same as Example 1, except that mulberry leaf extract is not added and is replaced with tea tree extract in an equal mass ratio.

[0058] Comparative Example 20

[0059] This comparative example is substantially the same as Example 1, except that no plant extract is added.

[0060] Comparative Example 21

[0061] The difference between this comparative example and Example 1 is that benzoic acid is not added, but ethylhexylglycerin of an equal mass ratio is used instead.

[0062] Comparative Example 22

[0063] The difference between this comparative example and Example 1 is that benzoic acid is not added, but 1,2-hexanediol is used in an equal mass ratio.

[0064] Comparative Example 23

[0065] The difference between this comparative example and Example 1 is that benzoic acid is not added, but octyl glycol in an equal mass ratio is used instead.

[0066] Effect evaluation test

[0067] The above Examples 1-12 and Comparative Examples 1-23 were subjected to a one-month stability test (stock solution at 4°C, room temperature, 55°C and 1% aqueous solution at room temperature), and the experimental results are recorded in Table 2.

[0068] Table 2 Stability of preservatives and fungicides

[0069]

[0070]

[0071] The stability test results of the above embodiments and comparative examples show that the present invention selects a mixed solvent system of water and alcohol to make the preservative and bactericidal product more stable. Using one of them alone will often lead to instability of the product and inconvenience in use. In addition, lauroyl arginine, benzalkonium chloride, polyaminopropyl biguanide, and cetylpyridinium chloride all have a certain solubilization effect, and the stability and water solubility of the products produced by different proportions will be different.

[0072] The antiseptics and bactericides prepared in the above Examples 1-12 and Comparative Examples 1-23 are respectively applied to wet wipes, and the specific methods are as follows:

[0073] (1) At room temperature, 2% glycerol, 1.5% alkyl glycoside, 0.5% preservative and bactericide, and the balance pure water are mixed according to mass percentage and stirred for 10-15 minutes, and then the pH is adjusted to between 4.5 and 6 with sodium hydroxide or sodium citrate to obtain wet wipes liquid.

[0074] (2) The pure cotton cloth is cut into the required size according to the target specifications, and then the wet wipes cloth and wet wipes liquid are sprayed or soaked in a machine according to a weight ratio of 1:3.6 to prepare the finished wet wipes. The water content of the wet wipes is controlled at 3.2 times.

[0075] According to GB 15979-2002 "Hygiene Standard for Disposable Sanitary Products", wet wipes to which the preservatives and bactericidal agents prepared in Examples 1-12 and Comparative Examples 3-6 and 8-23 were added were tested, and bactericidal tests were performed on Escherichia coli, Staphylococcus aureus, Candida albicans and Propionibacterium acnes, respectively. The experimental conditions were wet wipes as carriers, and the bactericidal action time was 2 minutes. The experimental results are shown in Table 3.

[0076] Table 3 Bactericidal test results

[0077]

[0078] According to Example 1 and Comparative Examples 3-6, at the same content, the bactericidal effect of the single-component antiseptic and bactericidal active ingredient in the wet wipes is worse than that of the mixed component. The possible reason is that the single component is easily adsorbed into the cotton fiber and is difficult to contact the bacteria completely. According to Example 1 and Comparative Examples 8-12, 15, 21-23, it can be seen that when any component of the antiseptic and bactericidal active ingredient is removed (one of the contents of lauroyl arginine ethyl ester hydrochloride, cetylpyridinium chloride, polyaminopropyl biguanide, benzalkonium chloride, and benzoic acid is 0) or any of the components is replaced with other antiseptic and synergistic ingredients, the bactericidal effect of the antiseptic and bactericidal agent prepared therefrom will be reduced or not stable enough. It can be seen from Example 1 and Comparative Examples 13-14, 16-20 that the jujube extract has a certain synergistic effect on the killing of Propionibacterium acnes, and Propionibacterium acnes is one of the causes of acne and local inflammation, so the jujube can synergistically enhance the effect and help relieve and improve the skin condition.

[0079] The content of each preservative and bactericidal agent in the wet wipes extrudate and the shredded wet wipes was detected by high performance liquid chromatography. The stability test results of the content of the preservative and bactericidal active ingredients of Examples 1-12 and Comparative Examples 3-6, 8-12, 15, 21-23 are shown in Table 4.

[0080] Table 4 Stability test results of the content of antiseptic and bactericidal active ingredients

[0081]

[0082]

[0083]

[0084] Note: ① In Table 4, “-” means that this component is not included in the solution, and the unit of each component is ppm;

[0085] ② The theoretical composition of each component from left to right in Example 1 is 750 ppm, 750 ppm, 50 ppm, 500 ppm, 500 ppm;

[0086] ③ In comparative examples 3-6, there is only a single component, and the theoretical value of the content is 2550 ppm;

[0087] ④ In Comparative Examples 21-23, ethylhexylglycerin, 1,2-hexanediol and caprylyl glycol were detected by gas chromatography. Due to the limitations of the detection method, the content results fluctuated greatly and could only be used as a reference for judgment. Therefore, detailed data are not listed here. After multiple data tests, it is generally judged that these three preservatives and synergists will not be absorbed by cotton fibers, and the contents in the extruded liquid are roughly equivalent to the theoretical values.

[0088] As can be seen from Table 4, in the wet wipes prepared in Example 1, the antiseptic and bactericidal active ingredients are evenly distributed in the wet wipes liquid and the wet wipes cloth, and can reach a concentration that effectively controls microorganisms, and can better protect the wet wipes. In Comparative Examples 3-6, the wet wipes prepared with only a single component of antiseptic and bactericidal ingredients have a low antiseptic content in the extruded liquid, and most of them are adsorbed by cotton fibers (wet wipes cloth). As can be seen from Comparative Examples 8-12 and 15, the order of adsorption strength of cotton fibers on several antiseptic and bactericidal active ingredients is: polyaminopropyl biguanide ≥ cetylpyridinium chloride > lauroyl arginine ethyl ester hydrochloride > benzalkonium chloride > benzoic acid. Among them, these ingredients can interact with cotton fibers and be adsorbed on them, so a "competitive effect" will be produced. In addition, benzoic acid can weaken the adsorption force of cotton fibers on the remaining four components, and ultimately make its active ingredients partially stably present in the wet wipes liquid, and this effect has little to do with the acid-base pH value. It can be seen from Example 1 and Comparative Examples 21-23 that ethylhexylglycerol, 1,2-hexanediol, and caprylyl glycol cannot weaken or affect the interaction between cotton fibers and the several antiseptic and bactericidal active ingredients selected in the present invention, and they themselves will not be adsorbed into the wet wipes.

[0089] The wet wipes added with the preservatives and bactericides prepared in the above-mentioned Examples 1-12 and Comparative Examples 3-6, 8-15, 21-23 were subjected to antiseptic challenge tests by two treatment methods: extrusion of liquid and shredding of wet wipes. The test method was based on "ASTM E640-2006 Test Method for Antiseptics of Water-Soluble Cosmetics". The specific results are shown in Tables 5 and 6.

[0090] Table 5 Results of the antiseptic challenge test of squeezed wet wipes

[0091]

[0092]

[0093] Table 6 Results of the antiseptic challenge test on shredded wet wipes

[0094]

[0095] Anticorrosion challenge microbial test strains:

[0096] Bacteria: Pseudomonas aeruginosa ATCC 9027

[0097] Escherichia coli ATCC 8739

[0098] Staphylococcus aureus ATCC 6538

[0099] Burkholderia cepacia ATCC 25416

[0100] Enterobacter gergoviae ATCC 33028

[0101] Fungi: Candida albicans ATCC 10231

[0102] Aspergillus niger ATCC 16404

[0103] Eupenicillium levitum ATCC 10464

[0104] It can be seen from Table 4, Table 5, and Table 6 that the wet wipes prepared with different raw material ratios have different adsorption strengths on the antiseptic and bactericidal active ingredients by cotton fibers, so the content of active substances distributed in the wet wipe liquid and wet wipe cloth is inconsistent, and their ability to prevent and control microorganisms is also different. Although most of them can pass the challenge, it takes a certain amount of time for the total colony count to be completely <10. Overall, the antiseptic effect will be weak, and the ability to resist microbial contamination risks will also be low. In particular, products with less active ingredients in the wet wipe liquid have poor antiseptic challenge data. Similarly, when antiseptic ingredients that are not easily adsorbed by cotton fibers are selected in the wet wipes, the active ingredients are all in the wet wipe liquid. At this time, there are no active ingredients in the cotton fibers, and the effect will be poor when doing the antiseptic challenge of cutting the wet wipes into pieces. From the data of comparative examples 21-23, it can be seen that although the ethylhexylglycerol, 1,2-hexanediol and caprylyl glycol we added additionally will not be adsorbed by the cloth, the effect is weak, so the antiseptic challenge result of the wet wipes liquid fails, and the bacterial antiseptic challenge data of the shredded wet wipes also needs 21 days to be completely <10, and these three antiseptic and synergistic ingredients all have a certain smell. When the amount added increases, it will affect the customer's experience. After the ratio of our Example 1 is optimized, the distribution of antiseptic and bactericidal active ingredients in the wet wipes liquid and wet wipes cloth can be effectively controlled, the microbial prevention and control capabilities of the two major sections of the wet wipes can be enhanced, and the shelf life of the wet wipes can be effectively extended.

[0105] The wet wipes liquid added with the preservatives and bactericides prepared in the above Examples 1-12 and Comparative Examples 13-14, 16-20 were tested for irritation according to SN / T 2329-2009 "Chicken Embryo Chorioallantoic Membrane Test for Eye Irritation / Corrosion of Cosmetics", and the reaction time method was used to conduct the test. The eye irritation of the test objects was classified according to Table 7 based on the calculated IS values. The specific irritation test data results are shown in Table 8:

[0106] Table 7 Evaluation of stimulation scoring method results

[0107]

[0108] Table 8 Test data results of wet wipes liquid chicken embryo allantoic membrane

[0109]

[0110] As can be seen from the above table, the irritation score of Example 1 is 0.12, which is non-irritating, while the scores of Comparative Examples 13-14 and 16-20 are also relatively low, but they are all mildly irritating. In addition, the jujube extract and mulberry leaf extract selected in the present invention have an obvious synergistic effect on mildness after being added to the formula, which can make the prepared wet wipes liquid more mild and non-irritating.

[0111] The wet wipes prepared by the above-mentioned Examples 1-12 and Comparative Examples 13-14, 16-20 were tested for use by volunteers, wherein the control group was wet wipes prepared with pure water (pH modulation between 5-6). The test method is: 114 volunteers were recruited and randomly divided into 19 groups, with 6 people in each group, and the volunteers were required to have no abnormal symptoms such as rashes and itching behind the ears and the inner side of the arms. Each group used the wet wipes of the test example (left) and the control example (right) at the same time, cut them into small pieces and attached them to the same position behind the ears and the inner side of the arms for 10 minutes, then removed the wet wipes and continued to observe the feelings for 20 minutes, and scored according to the skin condition and feelings of the volunteers after the trial, with 0 (no irritation)-9 (strong irritation / stinging) for scoring, and the average score was used as the final score. The specific test results are shown in Table 9.

[0112] Table 9 Volunteer test scores

[0113]

[0114] From the data in Table 9, it can be seen that the pattern is similar to that of the chicken embryo chorioallantoic membrane. Compared with the comparative examples, the Ziziphus jujuba extract and the mulberry leaf extract of Examples 1 to 12 can effectively enhance the mildness of the product.

[0115] In summary, the present invention can synergistically enhance the effectiveness of compounding the antiseptic and bactericidal active ingredients with water, butylene glycol, and plant extracts, thereby enhancing the bactericidal, antiseptic, and soothing effects of the antiseptic and bactericidal agent in the wet wipes, and improving its stability in the wet wipes system, thereby preventing microbial contamination caused by uneven distribution of the antiseptic and bactericidal active ingredients in the wet wipes liquid and the wet wipes cloth, resulting in insufficient antiseptic strength.

[0116] Those skilled in the art should recognize that the above embodiments are only used to illustrate the present invention, and are not intended to limit the present invention. As long as they are within the spirit of the present invention, various modifications as described above that are obvious to those skilled in the art to obtain the invention should be included in the scope of the claims of the present invention.

Claims

1. A method for preparing a mild, non-irritating and odorless preservative and bactericidal agent, characterized in that: Providing an antiseptic and fungicide active ingredient and a plant extract, mixing the antiseptic and fungicide active ingredient, the plant extract, butylene glycol and water, and preparing a mild, non-irritating and odorless antiseptic and fungicide after the mixture is completely dissolved; The antiseptic and bactericidal active ingredients are composed of lauroyl arginine ethyl ester hydrochloride, benzalkonium chloride, cetylpyridinium chloride, polyaminopropyl biguanide and benzoic acid, the plant extract is composed of jujube extract and mulberry leaf extract, and the mass ratio of benzalkonium chloride, polyaminopropyl biguanide, lauroyl arginine ethyl ester hydrochloride, cetylpyridinium chloride, benzoic acid, jujube extract, mulberry leaf extract, water and butylene glycol is (1-20): (1-20): (0.5-10): (1-20): (1-20): (1-8): (1-5): (10-25): (20-35); The preparation method of the jujube extract and the mulberry leaf extract is as follows: crushing the jujube and mulberry leaves respectively, then adding a 50% ethanol solution at a material-liquid mass ratio of 1: (15-20), performing ultrasonic extraction respectively, filtering after ultrasonic extraction, collecting the filtrate, repeating the above operation twice, combining the filtrate, evaporating and concentrating the filtrate under reduced pressure, and vacuum drying to obtain the jujube extract and the mulberry leaf extract.

2. The method for preparing the mild, non-irritating and odorless antiseptic and bactericidal agent according to claim 1, characterized in that: The following steps are involved: S10, preparing jujube extract and mulberry leaf extract; S20, mixing water and butanediol uniformly to obtain a mixed solution, and then adding benzalkonium chloride, polyaminopropyl biguanide, lauroyl arginine ethyl ester hydrochloride, benzoic acid, and cetylpyridinium chloride to the mixed solution in sequence, heating and stirring to obtain a colorless transparent solution; S30, adding the jujube extract and the mulberry leaf extract into the colorless transparent solution, stirring evenly, to prepare a mild, non-irritating and odorless preservative and bactericidal agent.

3. The method for preparing the mild, non-irritating and odorless antiseptic and bactericidal agent according to claim 2, characterized in that: The heating temperature in step S20 is 40°C to 60°C.

4. The method for preparing the mild, non-irritating and odorless antiseptic and bactericidal agent according to claim 2, characterized in that: The heating and stirring time in step S20 is 2 h to 4 h.

5. A mild, non-irritating and odorless preservative and bactericidal agent, characterized in that: The invention is prepared according to the method for preparing the mild, non-irritating and odorless preservative and bactericidal agent according to any one of claims 1 to 4.

6. A daily chemical product, characterized in that: The invention comprises an antiseptic and bactericide, wherein the antiseptic and bactericide is prepared by the preparation method of the mild, non-irritating and odorless antiseptic and bactericide according to any one of claims 1 to 4.

7. The daily chemical product according to claim 6, characterized in that: The daily chemical product is wet wipes liquid or wet wipes containing the wet wipes liquid.

Citation Information

Patent Citations

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