Plant composite multi-target synergistic antibacterial wet toilet paper and preparation method thereof

Abstract

The invention relates to the technical field of wet toilet paper, in particular to plant composite multi-target synergistic antibacterial wet toilet paper and a preparation method thereof, and the wet toilet paper is prepared by compounding wormwood fiber spunlace non-woven fabric and production liquid; the production liquid is prepared from the following raw materials in percentage by mass: 0.3 percent to 0.8 percent of capryloyl hydroximic acid, 0.02 percent to 0.08 percent of cetylpyridinium chloride, 1 percent to 3 percent of propylene glycol, 0.5 percent to 1 percent of CO40, 2.0 percent to 12.0 percent of a plant active compound, 0.01 percent to 0.06 percent of a pH regulator and the balance of electronic grade deionized water (EDI water), the sum of the mass percentages of the raw materials is 100%. The multi-target antibacterial wet toilet paper has the advantages that the multi-target antibacterial effect of the wet toilet paper is realized through the synergistic effect of the echinacea extract and the olive leaf extract in combination with the wormwood fiber base material; the preparation method of the wet toilet paper comprises a gradient extraction process and a technology of compounding with spraying under a certain dry-wet ratio, and the wet toilet paper has broad-spectrum bacteriostasis, is non-irritant, can be dispersed, and is suitable for sensitive skin and environment-friendly scenes.

Description

Technical Field

[0001] The present invention relates to the technical field of wet toilet paper, and in particular to a plant composite multi-target synergistic antibacterial wet toilet paper and a preparation method thereof. Background Art

[0002] In recent years, as consumers' demand for personal care products has increased, wet toilet paper, as a sanitary product that combines cleanliness, comfort and convenience, has gradually become the focus of market attention. Traditional wet toilet paper mostly uses synthetic fibers or non-woven fabrics as substrates, and relies on chemical additives in the formula to achieve functions such as sterilization and skin care. However, such products still have certain limitations in terms of environmental protection, skin friendliness and the application of natural ingredients. In this context, the research and development of functional materials using natural plant fibers as raw materials has become one of the innovation directions of the industry. Artemisia argyi fiber spunlace cloth stands out for its unique material properties - artemisia argyi, as a traditional medicinal plant, is rich in active ingredients such as volatile oils, flavonoids and polyphenols, and has natural antibacterial, anti-inflammatory and soothing effects. However, the antibacterial effect of artemisia argyi fiber is weaker than that of some chemical antibacterial agents, and it may not be able to completely inhibit the growth of pathogenic microorganisms in high humidity or severely polluted environments, and other ingredients are often needed to assist in its antibacterial effect.

[0003] Natural organic acids are extracted from plants, do not contain chemically synthesized ingredients, have no toxic side effects on the human body, are biodegradable, reduce environmental pollution, and achieve antibacterial properties by destroying bacterial cell membranes, inhibiting enzyme activity, or interfering with metabolic processes. They have excellent compatibility. However, their antibacterial activity is highly concentration-dependent, which may increase their irritation.

[0004] Therefore, finding suitable natural organic acids to use in combination with mugwort fiber to ensure light or no irritation on the basis of synergistic antibacterial effect is a difficult problem that needs to be solved urgently. Summary of the invention

[0005] The purpose of the present invention is to overcome the shortcomings of the prior art and provide a plant-composite multi-target synergistic antibacterial wet toilet paper and a preparation method thereof. The wet toilet paper achieves multi-target antibacterial through the synergistic effect of Echinacea extract, olive leaf extract, and caprylhydroxamic acid in combination with an wormwood fiber substrate; its preparation method includes a gradient extraction process and a technology of compounding with spraying at a certain dry-wet ratio, and the wet toilet paper of the present invention has broad-spectrum antibacterial, is non-irritating, and can be flushed, and is suitable for sensitive skin and environmental protection scenarios.

[0006] The present invention is achieved through the following technical solutions: on the one hand, a plant composite multi-target synergistic antibacterial wet toilet paper is provided, which is prepared based on a composite of wormwood fiber spunlace non-woven fabric and a production liquid; the raw materials of the production liquid, by mass percentage, include 0.3%-0.8% of octanoylhydroxamic acid, 0.02%-0.08% of cetylpyridinium chloride, 1%-3% of propylene glycol, 0.5%-1% of CO40, 2.0%-12.0% of a plant active compound, 0.01%-0.06% of a pH regulator, and the remainder is electronic grade deionized water (EDI water); and the sum of the mass percentages of the above raw materials is 100%.

[0007] Through the above technical scheme, Echinacea extract (main active ingredients chicoric acid and alkylamide) interferes with bacterial nucleic acid synthesis and blocks replication. Olive leaf extract (main active ingredients oleuropein and hydroxytyrosol) inhibits bacterial enzyme systems (such as ATPase and β-galactosidase) and interferes with energy metabolism. Wormwood fiber (main active ingredients eucalyptol and flavonoids): sustained release, releases volatile active ingredients, and destroys bacterial membrane permeability. Physically adsorbs bacteria to limit their movement and reproduction. The synergistic effect of the three not only covers a wider antibacterial spectrum, but also reduces the concentration of a single ingredient. At the same time, the inventor unexpectedly discovered that after adding caprylhydroxamic acid, it can not only cooperate with the system to inhibit bacteria, but also reduce the irritation caused by Echinacea extract and olive leaf extract.

[0008] The present invention makes it difficult for bacteria to survive through a single drug resistance mechanism through multi-target attacks, significantly improving the broad spectrum and efficiency of antibacterial activity. The porous fiber structure adsorbs and slowly releases antibacterial components to prolong the duration of action. The local component concentration is enhanced to improve the contact antibacterial effect. Hydroxytyrosol, an active ingredient in olive leaf extract, and phenolic acids, an active ingredient in echinacea extract, have strong antioxidant properties, can scavenge free radicals, reduce the defense response of bacteria due to oxidative stress, and reduce biofilm formation. The physical adsorption of wormwood fiber is combined with the chemical antibacterial effect of diols to form a double barrier. The fiber adsorbs bacteria and fixes their position, and the chemical components kill them directly. Prevent bacteria from reproducing after detachment, and achieve long-term antibacterial effect.

[0009] Preferably, the mass ratio of caprylhydroxamic acid, cetylpyridinium chloride, propylene glycol and CO40 is 1:0.2:4:2.

[0010] Furthermore, the plant active compound is compounded by echinacea extract and olive leaf extract; the mass ratio of echinacea extract to olive leaf extract is 1-6:1-6.

[0011] Furthermore, the preparation method of the Echinacea extract in the plant active compound is:

[0012] Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them and chop them into 15 mesh size;

[0013] Step 2: Mix the crushed raw material with 60% ethanol solution at a material-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 50-60°C under nitrogen protection, extract for 1.5h, then heat to 70-80°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter to separate the extract;

[0014] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes for decolorization, and filter to obtain a clarified liquid; concentrate the clarified liquid to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, and load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and elute impurities with deionized water (2 BV / h), elute the target component with 30% ethanol (2 BV / h), and collect the eluate.

[0015] Furthermore, the preparation method of the olive leaf extract in the plant active compound is:

[0016] Step 1: Select fresh olive leaves;

[0017] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0018] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, maintain enzymolysis at 40-60°C for 3-6 hours to obtain an enzymolysis solution; perform ultrasonic extraction on the enzymolysis solution for 0.5-1 hour; filter the enzymolysis solution obtained through the above steps through a filter membrane to obtain an olive leaf extract.

[0019] Furthermore, the wormwood fiber spunlace non-woven fabric is obtained by functionally treating the spunlace non-woven fabric with functional enhanced fibers; the functional enhanced fibers include wormwood staple fibers, wood pulp fibers, and lyocell fibers; the mass ratio of the wormwood staple fibers: wood pulp fibers: lyocell fibers is 1-3:12-14:3-7.

[0020] Through the above technical scheme, the steps of forming the wormwood spunlace fabric are to use functionally enhanced wormwood fiber, wood pulp, and viscose fiber for opening and mixing, combing into a web, cross-laying, pre-wetting, reinforcement, dehydration, drying, and shaping to obtain wormwood fiber spunlace non-woven fabric slices.

[0021] Also provided is a method for preparing the above-mentioned plant composite multi-target synergistic antibacterial wet toilet paper, comprising the following steps:

[0022] Step S1, preparing production liquid;

[0023] Add EDI water, caprylylhydroxamic acid, cetylpyridinium chloride, propylene glycol, CO40, plant active compound, and pH regulator in the above mass ratio in sequence and mix well, then stir for 25-35 minutes to obtain the production liquid;

[0024] Step S2: substrate forming

[0025] The spunlace nonwoven fabric is functionally treated with functional enhancing fibers to obtain wormwood fiber spunlace nonwoven fabric slices, and the slices are folded into square / rectangular / circular / special-shaped wet wipes;

[0026] Step S3: Composite packaging

[0027] The wet wipes are sprayed with the production liquid at a dry-wet ratio of 1:2, and are sealed and packaged using an OPP / VMPET / PE composite film under a sterile environment.

[0028] Furthermore, in step S1, the pH adjuster is one of sodium citrate and triethanolamine.

[0029] Furthermore, in step S2, the gram weight of the wormwood fiber spunlace nonwoven fabric slice is 70-80 g / m 2 The moisture content of the wet wipes after folding is ≤8%.

[0030] Furthermore, the antibacterial rates of the wet toilet paper against Staphylococcus aureus, Escherichia coli, and Candida albicans are 99.9%, 99.5%, and 95.5%, respectively.

[0031] Beneficial Effects

[0032] The wet toilet paper of the present invention achieves multi-target antibacterial effect through the synergistic effect of Echinacea extract, olive leaf extract, and caprylhydroxamic acid, combined with an wormwood fiber substrate; its preparation method includes a gradient extraction process and a spraying compound technology at a certain dry-wet ratio, and the wet toilet paper of the present invention has broad-spectrum antibacterial properties, is non-irritating, and can be flushed, and is suitable for sensitive skin and environmental protection scenarios.

[0033] The Echinacea extract (main active ingredients chicoric acid and alkylamide) of the present invention interferes with bacterial nucleic acid synthesis and blocks replication; the olive leaf extract (main active ingredients oleuropein and hydroxytyrosol) inhibits bacterial enzyme systems (such as ATPase and β-galactosidase) and interferes with energy metabolism; the wormwood fiber (main active ingredients eucalyptol and flavonoids) is slow-released, releases volatile active ingredients, destroys bacterial membrane permeability, and uses physical adsorption of bacteria to limit their movement and reproduction. The synergistic effect of the above three not only covers a wider antibacterial spectrum, but also reduces the use concentration of a single component. After adding octanoylhydroxamic acid at the same time, it can not only cooperate with the system to inhibit bacteria, but also reduce the irritation caused by the Echinacea extract and the olive leaf extract.

[0034] The present invention makes it difficult for bacteria to survive through a single drug resistance mechanism through multi-target attacks, significantly improving the broad spectrum and efficiency of antibacterial effect. The porous structure of the fiber adsorbs and slowly releases antibacterial components to prolong the duration of action. The local component concentration is enhanced to improve the contact antibacterial effect. Hydroxytyrosol, an active ingredient in olive leaf extract, and phenolic acids, an active ingredient in echinacea extract, have strong antioxidant properties, can scavenge free radicals, reduce the defense response of bacteria due to oxidative stress, and reduce biofilm formation. The physical adsorption of wormwood fiber is combined with the chemical antibacterial effect of diols to form a double barrier. The fiber adsorbs bacteria and fixes their position, and the chemical components kill them directly; it prevents bacteria from reproducing after detaching, and has long-lasting antibacterial effect. DETAILED DESCRIPTION

[0035] In order to make the purpose, technical solution and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not used to limit the present invention.

[0036] The present invention provides a method for preparing the above-mentioned plant composite multi-target synergistic antibacterial wet toilet paper, comprising the following steps:

[0037] Step S1, preparing production liquid;

[0038] Add EDI water, caprylylhydroxamic acid, cetylpyridinium chloride, propylene glycol, CO40, plant active compound, and pH regulator in the above mass ratio in sequence and mix well, then stir for 25-35 minutes to obtain the production liquid;

[0039] Step S2, substrate forming;

[0040] The spunlace nonwoven fabric is functionally treated with functional enhancing fibers to obtain wormwood fiber spunlace nonwoven fabric slices, and the slices are folded into square / rectangular / circular / special-shaped wet wipes;

[0041] Step S3, composite packaging;

[0042] The wet wipes are sprayed with the production liquid at a dry-wet ratio of 1:2, and are sealed and packaged using an OPP / VMPET / PE composite film under a sterile environment.

[0043] On the basis of the above scheme, the plant active complex is compounded by Echinacea purpurea extract and olive leaf extract;

[0044] Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. The experimental methods without specific conditions in the following examples are usually carried out under conventional conditions or according to the conditions recommended by the manufacturer. Unless otherwise specified, all percentages, ratios, proportions or parts are by weight.

[0045] Unless otherwise specified, the reagents and raw materials used in the examples and comparative examples of the present invention can be obtained through commercial channels.

[0046] Embodiment 1:

[0047] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.4% of octanoylhydroxamic acid, 0.08% of cetylpyridinium chloride, 1.5% of propylene glycol, 0.8% of CO40, 1% of echinacea extract, 1% of olive leaf extract, 0.05% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 5% wormwood fiber.

[0048] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0049] Step 2: Mix the crushed raw material with 60% ethanol solution at a material-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to the first stage temperature under nitrogen protection, extract for 1.5 hours, then heat to the second stage temperature, extract for 2 hours, then cool to the third stage temperature, cycle for 0.5 hours, and filter and separate to obtain the extract;

[0050] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and elute impurities with deionized water (2 BV / h), elute the target component with 30% ethanol (2 BV / h), and collect the eluate.

[0051] Step 4: Take the above extract and concentrate it to dryness under reduced pressure at 60℃, re-dissolve it with sterile PBS to 50mg / mL, filter it with 0.45μm filter membrane for sterilization and set aside. According to the antibacterial ring test method of GB 15979-2024E.6.4, the test strains are: Escherichia coli, Staphylococcus aureus, and Candida albicans.

[0052] Usually, the high-temperature extraction stage (second stage temperature) directly affects the yield of the active ingredients, and the low-temperature circulation stage directly affects the stability of the active ingredients. Therefore, the temperature changes of these two stages are as follows:

[0053]

[0054]

[0055] From the table above, we can see that when the temperature in the first stage is lower than 50℃, the temperature in the second stage is higher than 80℃ or lower than 70℃, and the temperature in the third stage is higher than 50℃, the yield and stability of Echinacea are affected, and the inhibitory effect on the three bacteria is weak. Comprehensively evaluating the inhibition rate of the three bacteria, the variable temperature condition of experimental group 1 was selected as the optimal condition.

[0056] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0057] Step 1: Select fresh olive leaves;

[0058] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0059] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 1.5-3% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 40-60°C for 3-6 hours to obtain an enzymolysis solution. Ultrasonic extraction is performed on the enzymolysis solution for 0.75 hours; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0060] Step 3: Each group of enzymatic hydrolysates were filtered through a 0.45 μm membrane, rotary evaporated at 60 °C for 2 h, and configured to 50 mg / mL. The test bacteria were Escherichia coli, Staphylococcus aureus, and Candida albicans according to the inhibition ring test method of GB15979-2024E.6.4.

[0061]

[0062]

[0063] The experimental results are shown in the following table:

[0064]

[0065] From the table above, we can see that olive extract has an inhibitory effect on the three bacteria, which is greatly affected by the enzymatic hydrolysis conditions. When the enzyme content is lower than 1.5%, the enzymatic hydrolysis temperature is lower than 40℃ or higher than 60℃, and the enzymatic hydrolysis time is lower than 3h, the inhibitory effect on the three bacteria is weak. The antibacterial effect of each experimental group was comprehensively evaluated, and experimental group 1 was selected as the optimal condition.

[0066] Embodiment 2:

[0067] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.4% of octanoylhydroxamic acid, 0.08% of cetylpyridinium chloride, 1.5% of propylene glycol, 0.8% of CO40, 2% of echinacea extract, 2% of olive leaf extract, 0.05% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0068] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0069] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 52°C under nitrogen protection, extract for 1.5h, then heat to 78°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0070] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0071] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0072] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0073] Step 1: Select fresh olive leaves;

[0074] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0075] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 45°C for 3.5 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0076] Embodiment three:

[0077] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.4% of octanoylhydroxamic acid, 0.08% of cetylpyridinium chloride, 1.5% of propylene glycol, 0.8% of CO40, 4% of echinacea extract, 4% of olive leaf extract, 0.05% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 11% wormwood fiber.

[0078] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0079] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 52°C under nitrogen protection, extract for 1.5h, then heat to 78°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0080] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir and decolorize at 53°C for 30 minutes, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and elute impurities with 5 BV of deionized water (2 BV / h), elute the target component with 6 BV of 30% ethanol (2 BV / h), and collect the eluate.

[0081] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0082] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0083] Step 1: Select fresh olive leaves;

[0084] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0085] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 52°C for 4 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0086] Embodiment 4:

[0087] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared by the above step S1 with 0.4% of octanoylhydroxamic acid, 0.08% of cetylpyridinium chloride, 1.5% of propylene glycol, 0.8% of CO40, 6% of echinacea extract, 6% of olive leaf extract, 0.03% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 15% wormwood fiber.

[0088] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0089] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 59°C under nitrogen protection, extract for 1.5h, then heat to 73°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0090] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0091] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0092] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0093] Step 1: Select fresh olive leaves;

[0094] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0095] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 50°C for 4 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0096] Embodiment five:

[0097] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by containing 0.35% of octanoylhydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 1% of echinacea extract, 2% of olive leaf extract, 0.03% of sodium citrate, and the remainder of EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 11% wormwood fiber.

[0098] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0099] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 60°C under nitrogen protection, extract for 1.5h, then heat to 75°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0100] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0101] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0102] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0103] Step 1: Select fresh olive leaves;

[0104] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0105] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 45°C for 4 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0106] Embodiment six:

[0107] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.35% of octanoylhydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 2% of echinacea extract, 1% of olive leaf extract, 0.03% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 15% wormwood fiber.

[0108] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0109] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 50°C under nitrogen protection, extract for 1.5h, then heat to 75°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0110] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0111] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0112] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0113] Step 1: Select fresh olive leaves;

[0114] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0115] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 50°C for 3.5 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0116] Embodiment seven:

[0117] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by containing 0.35% of octanoylhydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 4% of echinacea extract, 6% of olive leaf extract, 0.03% of sodium citrate, and the remainder of EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 5% wormwood fiber.

[0118] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0119] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 59°C under nitrogen protection, extract for 1.5h, then heat to 70°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0120] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0121] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0122] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0123] Step 1: Select fresh olive leaves;

[0124] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0125] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 48°C for 5 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0126] Embodiment eight:

[0127] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by containing 0.35% of octanoylhydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 6% of echinacea extract, 4% of olive leaf extract, 0.03% of sodium citrate, and the remainder of EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0128] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0129] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 55°C under nitrogen protection, extract for 1.5h, then heat to 75°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0130] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0131] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0132] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0133] Step 1: Select fresh olive leaves;

[0134] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0135] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 50°C for 4 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0136] Embodiment nine:

[0137] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.8% of octanoylhydroxamic acid, 0.03% of cetylpyridinium chloride, 2% of propylene glycol, 1% of CO40, 1% of echinacea extract, 4% of olive leaf extract, 0.06% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 15% wormwood fiber.

[0138] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0139] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 54°C under nitrogen protection, extract for 1.5h, then heat to 75°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0140] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0141] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0142] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0143] Step 1: Select fresh olive leaves;

[0144] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0145] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 56°C for 3.5 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0146] Embodiment ten:

[0147] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.8% of octanoylhydroxamic acid, 0.03% of cetylpyridinium chloride, 2% of propylene glycol, 1% of CO40, 2% of echinacea extract, 6% of olive leaf extract, 0.06% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 11% wormwood fiber.

[0148] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0149] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 52°C under nitrogen protection, extract for 1.5h, then heat to 70°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0150] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0151] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0152] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0153] Step 1: Select fresh olive leaves;

[0154] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0155] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 60°C for 5 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0156] Embodiment eleven:

[0157] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by containing 0.8% of octanoylhydroxamic acid, 0.03% of cetylpyridinium chloride, 2% of propylene glycol, 1% of CO40, 4% of echinacea extract, 1% of olive leaf extract, 0.06% of sodium citrate, and the remainder of EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0158] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0159] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 60°C under nitrogen protection, extract for 1.5 hours, then heat to 60°C, extract for 2 hours, then cool to below 50°C, circulate for 0.5 hours, and filter and separate to obtain the extract.

[0160] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0161] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0162] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0163] Step 1: Select fresh olive leaves;

[0164] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0165] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 45°C for 5 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0166] Embodiment 12:

[0167] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by containing 0.8% of octanoylhydroxamic acid, 0.03% of cetylpyridinium chloride, 2% of propylene glycol, 1% of CO40, 6% of echinacea extract, 2% of olive leaf extract, 0.06% of sodium citrate, and the remainder of EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 5% wormwood fiber.

[0168] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0169] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 52°C under nitrogen protection, extract for 1.5h, then heat to 80°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0170] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0171] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0172] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0173] Step 1: Select fresh olive leaves;

[0174] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0175] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 60°C for 3 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0176] Embodiment 13:

[0177] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by containing 0.5% of octanoylhydroxamic acid, 0.02% of cetylpyridinium chloride, 3% of propylene glycol, 0.6% of CO40, 1% of echinacea extract, 6% of olive leaf extract, 0.04% of sodium citrate, and the remainder of EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0178] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0179] Step 2: Mix the crushed raw material with 60% ethanol solution at a material-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 55°C under nitrogen protection, extract for 1.5h, then heat to 80°C, extract for 2h, cool to below 50°C, cycle for 0.5h, and filter to separate the extract.

[0180] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0181] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0182] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0183] Step 1: Select fresh olive leaves;

[0184] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0185] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 60°C for 3 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0186] Embodiment 14:

[0187] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.5% of octanoylhydroxamic acid, 0.02% of cetylpyridinium chloride, 3% of propylene glycol, 0.6% of CO40, 2% of echinacea extract, 4% of olive leaf extract, 0.04% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 5% wormwood fiber.

[0188] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0189] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 50°C under nitrogen protection, extract for 1.5h, then heat to 80°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0190] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0191] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0192] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0193] Step 1: Select fresh olive leaves;

[0194] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0195] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 60°C for 6 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0196] Embodiment 15:

[0197] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.5% of octanoylhydroxamic acid, 0.02% of cetylpyridinium chloride, 3% of propylene glycol, 0.6% of CO40, 4% of echinacea extract, 2% of olive leaf extract, 0.04% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 15% wormwood fiber.

[0198] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0199] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 57°C under nitrogen protection, extract for 1.5h, then heat to 71°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0200] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0201] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0202] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0203] Step 1: Select fresh olive leaves;

[0204] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0205] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 44°C for 4 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0206] Embodiment 16:

[0207] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.5% of octanoylhydroxamic acid, 0.02% of cetylpyridinium chloride, 3% of propylene glycol, 0.6% of CO40, 6% of echinacea extract, 1% of olive leaf extract, 0.04% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 11% wormwood fiber.

[0208] Specifically, the preparation process of Echinacea extract is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them, and chop them into 15 mesh size.

[0209] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 55°C under nitrogen protection, extract for 1.5h, then heat to 80°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0210] Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes to decolorize, and filter to obtain a clear solution. Concentrate the clear solution to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and use 5 BV of deionized water (2 BV / h) to elute impurities, 6 BV of 30% ethanol (2 BV / h) to elute the target component, and collect the eluate.

[0211] Step 4: After the eluate is concentrated, adjust the pH to 2.0-3.0 and set aside.

[0212] Specifically, the method for extracting olive leaf extract comprises the following steps:

[0213] Step 1: Select fresh olive leaves;

[0214] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0215] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 45°C for 5 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0216] Effect embodiment 1:

[0217] The irritation of Examples 1 to 16 was tested respectively.

[0218] Antibacterial rate: According to the antibacterial performance test method operating procedures of C4 dissolution antibacterial product in Appendix C of GB15979-2002 "Sanitary Standards for Disposable Hygiene Products", the antibacterial efficacy of the samples against Escherichia coli, Staphylococcus aureus and Candida albicans was examined. Evaluation criteria:

[0219] The antibacterial rate is ≥50% to 90%, and the product has an antibacterial effect;

[0220] The antibacterial rate is ≥90%, and the product has a strong antibacterial effect.

[0221] The results of the antibacterial rate of the embodiment are shown in the following table

[0222] Examples / Projects Escherichia coli Staphylococcus aureus Candida albicans Embodiment 1 90.18％ 82.53％ 50.35％ Embodiment 2 99.9％ 99％ 86.12％ Embodiment 3 99.5％ 99.9％ 90.45％ Embodiment 4 99.9％ 99.9％ 99.11％ Embodiment 5 98.32％ 99％ 73.25％ Embodiment 6 98.63％ 99％ 75.33％ Embodiment 7 99.9％ 99％ 88.42％ Embodiment 8 99.9％ 99.9％ 95.53％ Embodiment 9 98.23％ 99％ 72.44％ Embodiment 10 97.89％ 99％ 85.33％ Embodiment 11 96.57％ 99％ 82.79％ Embodiment 12 99.9％ 99％ 88.69％ Embodiment 13 92.12％ 95.65％ 64.32％ Embodiment 14 98.35％ 99％ 76.58％ Embodiment 15 99.9％ 99％ 85.33％ Embodiment 16 99.9％ 99％ 91.22％

[0223] According to the experimental results, the best combination is Example 4. Since the cost of the wormwood fiber spunlace cloth in this combination is relatively high, there is no significant difference in the antibacterial rate compared with Example 8. Comprehensive consideration leads to the best combination Example 8.

[0224] Comparative Example 1: No preservatives added

[0225] A plant composite multi-target synergistic antibacterial wet toilet paper, comprising a production liquid and a flushable spunlace non-woven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 with 1% echinacea extract, 1% olive leaf extract, 0.05% sodium citrate, and the remainder being EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0226] Comparative Example 2: No Echinacea Extract Added

[0227] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.35% of octanoylhydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 4% of olive leaf extract, 0.03% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0228] Comparative Example 3: No olive leaf extract added

[0229] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by containing 0.35% of octanoylhydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 6% of echinacea extract, 0.03% of sodium citrate and the remainder of EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0230] Comparative Example 4: Spunlace fabric can be dispersed without adding wormwood fiber

[0231] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.35% of octanoylhydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 6% of echinacea extract, 4% of olive leaf extract, 0.03% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are ordinary flushable spunlace fabrics.

[0232] Comparative Example 5: Chamomile extract replaces Echinacea extract

[0233] A plant composite multi-target synergistic antibacterial wet toilet paper, comprising a production liquid and a spunlace nonwoven fabric containing wormwood fiber that can be dispersed; wherein the production liquid is prepared according to the above step S1 by 0.35% of octanoyl hydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 6% of chamomile extract, 4% of olive leaf extract, 0.03% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are 8% wormwood fiber content spunlace nonwoven fabric

[0234] Comparative Example 6: Replacement of olive leaf extract with olive leaf extract

[0235] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.35% of octanoylhydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 6% of echinacea extract, 4% of olive leaf extract, 0.03% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0236] Comparative Example 7: EDTA-2Na replaces octanoylhydroxamic acid

[0237] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.35% EDTA-2Na, 0.06% cetylpyridinium chloride, 1% propylene glycol, 0.5% CO40, 6% echinacea extract, 4% olive leaf extract, 0.03% sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0238] Comparative Example 8: Changing the temperature of the extraction process of Echinacea extract

[0239] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.35% of octanoylhydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 6% of echinacea extract, 4% of olive leaf extract, 0.03% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0240] The temperature of the extraction process of Echinacea extract was changed. Specifically, the preparation process of Echinacea extract was as follows: Step 1: Select Echinacea plants grown for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them and chop them into 15 mesh size.

[0241] Step 2: Mix the crushed raw material with 60% ethanol solution at a solid-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 40°C under nitrogen protection, extract for 1.5h, then heat to 90°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter and separate to obtain the extract.

[0242] Comparative Example 9: Changing the olive leaf extraction process and enzymatic hydrolysis conditions

[0243] A plant composite multi-target synergistic antibacterial wet toilet paper comprises a production liquid and a flushable spunlace nonwoven fabric containing wormwood fiber; wherein the production liquid is prepared according to the above step S1 by 0.35% of octanoylhydroxamic acid, 0.06% of cetylpyridinium chloride, 1% of propylene glycol, 0.5% of CO40, 6% of echinacea extract, 4% of olive leaf extract, 0.03% of sodium citrate, and the remainder is EDI pure water; and the wet toilet paper is prepared according to steps S2 and S3, and the wet wipes used are flushable spunlace fabrics containing 8% wormwood fiber.

[0244] Specifically, the olive leaf extraction process and enzymatic hydrolysis conditions are changed, comprising the following steps:

[0245] Step 1: Select fresh olive leaves;

[0246] Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water;

[0247] Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, and the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, and keep the enzymolysis at 70°C for 2 hours to obtain an enzymolysis solution. The enzymolysis solution is subjected to ultrasonic extraction for 30 minutes to 1 hour; the enzymolysis solution obtained through the above steps is filtered through a filter membrane to obtain an olive leaf extract.

[0248] Effect embodiment 2:

[0249] Experimental steps: The irritation of the compositions of Example 8 and Comparative Examples 1-9 was tested respectively.

[0250] The specific test method is: refer to the "Chicken Embryo Chorioallantoic Membrane Test for Eye Irritation / Corrosion of Cosmetics" (SN / T2329-2009), and the test adopts the reaction time method. Take 9-day-old SPF-grade chicken embryos for egg inspection, remove the eggshell at the top of the air chamber, and expose the chorioallantoic membrane (CAM). Take 0.3mL of the test substance and drip it directly on the surface of the CAM, observe and record the time when bleeding, vascular melting, and coagulation begin within 5 minutes. Each test substance is subjected to 6 parallel experiments. At the same time, set up a negative control (0.9% sodium chloride injection by mass) and a positive control (0.1mol / L sodium hydroxide solution). According to the formula:

[0251] IS = (301-secH) x 5 / 300 + (301-secL) x 7 / 300 + (301-secC) x 9 / 300. The stimulation score was calculated.

[0252] Where: secH is the average time for bleeding to start on the CAM membrane, in seconds (s); secL is the average time for vascular melting to start on the CAM membrane, in seconds (s); secC is the average time for coagulation to start on the CAM membrane, in seconds (s). Irritation classification: IS < 1, no irritation; 1 ≤ IS < 5, mild irritation; 5 ≤ IS < 9, moderate irritation; IS ≥ 9, strong irritation.

[0253]

[0254]

[0255] From Comparative Examples 1-4, it can be concluded that only when the preservative ingredients, echinacea extract, olive leaf extract and wormwood fiber spunlace cloth of the invention coexist, can a better antibacterial effect be achieved. From Comparative Examples 5-9, it can be concluded that when the echinacea extract, olive leaf extract and caprylhydroxamic acid in the invention are replaced with ingredients with the same efficacy, the original antibacterial effect cannot be achieved, and the antibacterial effect of the echinacea extract can only be exerted when the temperature in the echinacea extraction process is 50-80°C. It can be seen from Example 8 and Comparative Examples 1 and 7 that the irritation is medium when caprylhydroxamic acid is missing and replaced, indicating that caprylhydroxamic acid can reduce the irritation caused by plant extracts in this system.

[0256] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A plant-composite multi-target synergistic antibacterial wet toilet paper, characterized in that: The wet toilet paper is prepared by compounding wormwood fiber spunlace non-woven fabric with production liquid; the raw materials of the production liquid, calculated by mass percentage, include 0.3%-0.8% of octanoylhydroxamic acid, 0.02%-0.08% of cetylpyridinium chloride, 1%-3% of propylene glycol, 0.5%-1% of CO40, 2.0%-12.0% of plant active compound, 0.01%-0.06% of pH regulator, and the balance is electronic grade deionized water (EDI water); and the sum of the mass percentages of the above raw materials is 100%.

2. The plant composite multi-target synergistic antibacterial wet toilet paper according to claim 1, characterized in that: The plant active compound is compounded by echinacea extract and olive leaf extract; the mass ratio of the echinacea extract to the olive leaf extract is 1-6:1-6.

3. The plant composite multi-target synergistic antibacterial wet toilet paper according to claim 2, characterized in that: The preparation method of the Echinacea extract in the plant active compound is as follows: Step 1: Select Echinacea plants that have been planted for 1-3 years, collect the above-ground parts (stems, leaves) and roots, wash them and chop them into 15 mesh size; Step 2: Mix the crushed raw material with 60% ethanol solution at a material-liquid ratio of 1:10 (m / v), add 0.2% citric acid as a stabilizer, heat to 50-60°C under nitrogen protection, extract for 1.5h, then heat to 70-80°C, extract for 2h, then cool to below 50°C, circulate for 0.5h, and filter to separate the extract; Step 3: Add 1.5% activated carbon (w / v) to the filtrate, stir at 50°C for 30 minutes for decolorization, and filter to obtain a clarified liquid; concentrate the clarified liquid to a density of 1.12 g / mL (60°C), adjust the pH to 3.0, and load it onto an AB-8 macroporous resin column at a flow rate of 4 BV / h, and elute impurities with deionized water (2 BV / h), elute the target component with 30% ethanol (2 BV / h), and collect the eluate.

4. The plant composite multi-target synergistic antibacterial wet toilet paper according to claim 2, characterized in that: The preparation method of the olive leaf extract in the plant active compound is as follows: Step 1: Select fresh olive leaves; Soak the selected olive leaves in salt water for 1 to 2 hours, then rinse with clean water; Step 2: Use a high-speed wall-breaking machine to break the washed olive leaves at a temperature below room temperature; add 5 times water to the broken olive leaves, add cellulase, the amount of cellulase is 2% of the raw material in terms of mass / volume fraction, maintain enzymolysis at 40-60°C for 3-6 hours to obtain an enzymolysis solution; perform ultrasonic extraction on the enzymolysis solution for 0.5-1 hour; filter the enzymolysis solution obtained through the above steps through a filter membrane to obtain an olive leaf extract.

5. The plant composite multi-target synergistic antibacterial wet toilet paper according to claim 1, characterized in that: The wormwood fiber spunlace nonwoven fabric is obtained by functionally treating the spunlace nonwoven fabric with functional enhancement fibers; the functional enhancement fibers include wormwood staple fibers, wood pulp fibers, and lyocell fibers; the mass ratio of the wormwood staple fibers: wood pulp fibers: lyocell fibers is 1-3:12-14:3-7.

6. A method for preparing the plant composite multi-target synergistic antibacterial wet toilet paper according to any one of claims 1 to 5, characterized in that: The following steps are involved: Step S1, preparing production liquid; Add EDI water, caprylylhydroxamic acid, cetylpyridinium chloride, propylene glycol, CO40, plant active compound, and pH regulator in the above mass ratio in sequence and mix well, then stir for 25-35 minutes to obtain the production liquid; Step S2, substrate forming; The spunlace nonwoven fabric is functionally treated with functional enhancing fibers to obtain wormwood fiber spunlace nonwoven fabric slices, and the slices are folded into square / rectangular / circular / special-shaped wet wipes; Step S3, composite packaging; The wet wipes are sprayed with the production liquid at a dry-wet ratio of 1:2, and are sealed and packaged using an OPP / VMPET / PE composite film under a sterile environment.

7. The method for preparing the plant composite multi-target synergistic antibacterial wet toilet paper according to claim 6, characterized in that: In step S1, the pH adjuster is one of sodium citrate and triethanolamine.

8. The method for preparing the plant composite multi-target synergistic antibacterial wet toilet paper according to claim 7, characterized in that: In step S2, the gram weight of the wormwood fiber spunlace nonwoven fabric slice is 70-80 g / m 2 The moisture content of the wet wipes after folding is ≤8%.

9. The plant composite multi-target synergistic antibacterial wet toilet paper according to any one of claims 1 to 5, characterized in that: The antibacterial rates of the wet toilet paper against Staphylococcus aureus, Escherichia coli and Candida albicans are 99.9%, 99.5% and 95.5% respectively.

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