Environment-friendly antibacterial composition as well as preparation method and application thereof

Abstract

The invention relates to an environment-friendly antibacterial composition as well as a preparation method and application thereof. The environment-friendly antibacterial composition comprises an antibacterial enzyme, a stabilizer, an organic antibacterial agent, an anti-mite agent, a solubilizer and a coupling agent, and specifically comprises the following components in percentage by weight: 3-5% of lysozyme, 1-2% of dimethyl octadecyl [3-(trimethoxysilyl) propyl] ammonium chloride, 1-3% of octadecyl hydroxypropyl sulfobetaine, 2-4% of chitosan quaternary ammonium salt and the balance of water. The antibacterial composition is prepared from the following components in percentage by weight: 0.5 to 2 percent of sodium alginate, 0.5 to 1.5 percent of eugenol, 0.5 to 1 percent of sophocarpidine, 1 to 2 percent of PEG-60 hydrogenated castor oil, 0.5 to 1 percent of 3-aminopropyltrimethoxysilane and the balance of deionized water, the antibacterial enzyme, the organic antibacterial agent and the anti-mite agent can synergistically improve the antibacterial and anti-mite effects of the composition, and the antibacterial composition is strong in binding force with textiles, good in anti-mite effect, good in antibacterial effect, good in anti-mite effect and good in anti-mite effect. The textile prepared by taking the antibacterial composition as an effective component has the characteristics of washing resistance and excellent stability, and also has remarkable antibacterial long-term effect and relatively strong anti-mite effect.

Description

Technical Field

[0001] The present invention relates to the technical field of textile auxiliaries, and in particular to an environmentally friendly antibacterial composition and a preparation method and application thereof. Background Art

[0002] As consumers' awareness of health protection increases, textile finishing processes such as antibacterial, mildew-proof and anti-mite have attracted more attention, and people are more eager for healthy and safe textiles. At present, the commonly used antibacterial additives in textiles are roughly divided into three categories according to their composition: inorganic antibacterial agents, organic antibacterial agents and natural antibacterial agents. Inorganic antibacterial agents may cause certain toxic risks to the human body and the environment. Although organic antibacterial agents have strong bactericidal ability and good color stability, they have poor heat resistance, are easy to precipitate in solvent environments, and have poor stability. Natural antibacterial agents are green and non-toxic, but they are difficult to process, have poor heat resistance, short service life and high cost.

[0003] The use of a single antimicrobial agent may also have problems such as narrow antimicrobial spectrum, poor heat resistance, and easy drug resistance. Patent CN105019236A discloses a composite antimicrobial finishing agent for textiles, including polyhexamethylene guanidine, betaine, nano zinc oxide, chitosan, surfactant, organic solvent and essence; Patent CN105625039A discloses an environmentally friendly antibacterial, mildew-proof and mite-repellent fabric finishing agent, including polyhexamethylene biguanide and aloin, and anti-mite finishing aids are mountain briar seed oil and eugenol; Patent CN107794755A discloses an antibacterial deodorant and its preparation method, the antibacterial deodorant includes nano zinc oxide, ammonium chloride, chitosan, pollen, polyhexamethylene guanidine, triethanolamine, fennel, tea tree oil, sodium dodecylbenzene sulfonate and ethanol. Most of the antimicrobial agents for fabrics in the above inventions contain metal antimicrobial agents or have poor antibacterial effects and washing resistance. In addition, for antimicrobial agents for textiles, in addition to requiring good antimicrobial properties, attention should also be paid to the adhesion of the antimicrobial agents to ensure their long-lasting antibacterial properties while the physical properties of the textiles themselves, such as strength and breathability, are not affected.

[0004] In view of the deficiencies in the prior art, the present invention provides an environmentally friendly antibacterial composition for textiles, which has a broad spectrum and high efficiency, good biocompatibility and safety, is non-irritating, has long-lasting antibacterial and anti-mite effects, improves antibacterial performance and scope of application, and has the advantages of high heat resistance, high stability, good safety, high antibacterial efficiency and good anti-mite effect. Summary of the invention

[0005] In order to solve the above problems, the present invention first provides an environmentally friendly antibacterial composition, which comprises an antibacterial enzyme, a stabilizer, an organic antibacterial agent, an anti-mite agent, a solubilizer and a coupling agent, including the following mass percentages: antibacterial enzyme 0.2%-20%, organic antibacterial agent 2%~30%, stabilizer 0.5%~10%, anti-mite agent 0.5%~10%, solubilizer 1%~20%, coupling agent 0.5%~5%, and the balance is deionized water.

[0006] Furthermore, in terms of mass percentage, it includes: antimicrobial enzyme: 3% to 5%; organic antimicrobial agent: 5% to 8%; stabilizer: 0.5% to 2%; anti-mite agent: 1% to 2.5%; solubilizer: 1% to 2%; coupling agent: 0.5% to 1%; and the balance: deionized water.

[0007] Further, the antimicrobial enzyme may include one or a combination of lysostaphin, subtilisin, bacteriophage lyase, lysozyme, alginate lyase, glucose oxidase, cellobiose dehydrogenase, lactoperoxidase, and myeloperoxidase;

[0008] Furthermore, the stabilizer includes one or a combination of alginic acid, alginate, sodium dextran phosphate, gelatin, xanthan gum, sodium polyacrylate, polyacrylate, polyvinyl alcohol, polyvinyl pyrrolidone, polybetaine, vinylimidazole polymer, and polyethyleneimine.

[0009] Further, the organic antimicrobial agent may include synthetic organic antimicrobial agents (such as guanidine salts, quaternary ammonium salts, betaine antimicrobial agents) and natural or naturally modified organic antimicrobial agents (such as lignin, chitosan and its derivatives). The anti-mite agent may include one of eugenol, eucalyptus leaf extract, tea tree oil, matrine, geraniol, lavender oil, cinnamon oil or a combination thereof;

[0010] Furthermore, the solubilizer can be selected from one or a combination of PEG-60 hydrogenated castor oil, polyglyceryl-2 triisostearate, propylene glycol, hexylene glycol, isohexylene glycol, caprylyl glycol and polyethylene glycol; the coupling agent can be selected from one or a combination of vinyl silane, aminosilane, epoxy silane and mercapto silane to enhance the bonding force between the composition and cotton fiber and improve its stability.

[0011] In certain embodiments, the environmentally friendly antibacterial composition provided by the present invention achieves efficient inhibition and repellency of bacteria and mites through the synergistic effect of multiple antibacterial ingredients, has broad-spectrum antibacterial ability, is washable, and is environmentally friendly and harmless.

[0012] Among them, the addition of lysozyme gives the composition an enzymatic effect, allowing it to destroy bacterial cell walls and further enhance the antibacterial effect; organic antibacterial agents such as chitosan quaternary ammonium salts and dimethyloctadecyl [3-(trimethoxysilyl)propyl] ammonium chloride provide lasting antibacterial effects, and at the same time synergize with plant extract anti-mite agents to achieve the purpose of efficient anti-mite; stabilizers such as sodium alginate help maintain the stability of the system, so that the antibacterial components are evenly distributed and the use effect is improved; coupling agents enhance the binding force between the antibacterial components and cotton fibers by chemical bonding, thereby improving the water resistance and long-term stability of the coating.

[0013] The present invention also provides a method for preparing an antibacterial cotton fabric, the method comprising the following steps:

[0014] Pretreatment of cotton fabric: wash the cotton fabric to remove surface grease and impurities, and dry it for later use; preparation of environmentally friendly antibacterial composition: prepare the environmentally friendly antibacterial composition according to the above formula ratio and stir it evenly; impregnation treatment: soak the cotton fabric in the antibacterial composition solution to ensure that the fiber evenly absorbs the antibacterial component; cross-linking fixation: dry the soaked cotton fabric to firmly bind the antibacterial component to the fiber surface; final finishing: after cooling, a washable, antibacterial and anti-mite cotton fabric is obtained.

[0015] Finally, the present invention provides an application of an environmentally friendly antibacterial composition in antibacterial and anti-mite textiles, which is specifically used in the fields of cotton fabrics, bedding, medical textiles, sanitary products, sportswear, etc., to give textiles long-lasting antibacterial and anti-mite properties. The treated cotton fabric has excellent water washability. After 150 washes, it can still maintain the 7A antibacterial level, and the mite repellency rate is ≥80%, showing long-term and stable antibacterial and anti-mite performance.

[0016] In some embodiments, the environmentally friendly antibacterial composition is suitable for spraying, dipping, padding or other industrial coating processes, and can give the fabric excellent antibacterial properties without affecting the comfort and breathability of the fabric. After optimizing the combination formula and preparation process, the antibacterial finishing agent can be widely used in many fields such as home furnishing, medical treatment, and clothing.

[0017] Compared with the prior art, the present invention has at least the following beneficial effects:

[0018] Highly effective and broad-spectrum antibacterial: The lysozyme, organic antibacterial agent and anti-mite agent in the composition work synergistically, so that the treated textiles have significant inhibitory and repellent effects on bacteria, fungi and mites, with an antibacterial rate of more than 99%.

[0019] Strong resistance to water washing: Through the action of coupling agents (such as 3-aminopropyltrimethoxysilane), the antibacterial ingredients are chemically bonded to the cotton fibers to enhance the binding force, so that the antibacterial effect can remain stable after multiple washings.

[0020] Environmentally friendly and safe: The ingredients used are food-grade enzymes, plant extracts and harmless antibacterial agents. They do not contain harmful heavy metals or organic solvents, meet environmental protection requirements, and are non-irritating to the human body.

[0021] Wide range of applications: The antibacterial composition can be applied to various types of textiles, including household items, clothing, medical textiles, etc. It can be processed by various methods such as padding, dipping, spraying, etc., and has strong process adaptability.

[0022] Long-term stability: The antibacterial test and the water washing experiment verified that the antibacterial cotton fabric of the present invention can still maintain the antibacterial effect after 150 times of water washing, and has good mite repelling ability.

[0023] The present invention utilizes silane coupling agent for the first time to enhance the bonding between antibacterial agent and cotton fiber, forms a stable chemical bond through Si-OC bond, improves the stability of antibacterial coating, and significantly enhances the long-term antibacterial and anti-mite effect of textiles.

[0024] The present invention is the first to synergistically apply lysozyme, quaternary ammonium salt, chitosan quaternary ammonium salt, plant anti-mite agent and silane coupling agent to the field of antibacterial finishing of cotton fabrics, and successfully prepares environmentally friendly antibacterial cotton fabrics that are washable, long-lasting and antibacterial and anti-mite. Compared with the existing antibacterial finishing technology, the antibacterial composition of the present invention has stronger binding force, better antibacterial durability, and avoids the drug resistance problem that may be caused by traditional antibacterial agents, which is in line with the current development trend of green and environmentally friendly textiles. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 Antibacterial activity test of environmentally friendly antibacterial composition.

[0026] Figure 2 Characterization of lysozyme by fluorescence labeling to analyze the binding effect of antibacterial cotton fiber samples. DETAILED DESCRIPTION

[0027] In order to make the technical problems, technical solutions and advantages to be solved by the present invention more clear, a detailed description will be given below with reference to the accompanying drawings and specific embodiments.

[0028] Example 1: An environmentally friendly antibacterial composition, composed of the following mass percentages, lysozyme (CAS: 12650-88-3) 3%, dimethyl octadecyl [3- (trimethoxysilyl) propyl] ammonium chloride (CAS No.: 27668-52-6) 1%, octadecyl hydroxypropyl sulfobetaine (DY-OHSB) 1%, chitosan quaternary ammonium salt 2%, sodium alginate 0.5%, eugenol 0.5%, matrine 0.5%, PEG-60 hydrogenated castor oil 1%, 3-aminopropyl trimethoxysilane 1%, and the balance is deionized water; wherein chitosan quaternary ammonium salt was purchased from Shanghai Bide Pharmaceutical Technology Co., Ltd. (Article No.: BD02625758 Chitosanquaternary ammonium salt, 97%), and octadecyl hydroxypropyl sulfobetaine (DY-OHSB) was purchased from Shanghai Deyi Chemical Co., Ltd.;

[0029] Example 2: An environmentally friendly antibacterial composition, composed of the following mass percentages, lysozyme (CAS: 12650-88-3) 5%, dimethyl octadecyl [3- (trimethoxysilyl) propyl] ammonium chloride (CAS No.: 27668-52-6) 2%, octadecyl hydroxypropyl sulfobetaine (DY-OHSB) 2%, chitosan quaternary ammonium salt 4%, sodium alginate 1.5%, eugenol 1%, matrine 1%, PEG-60 hydrogenated castor oil 1.5%, 3-aminopropyl trimethoxysilane 0.5%, and the balance is deionized water; wherein chitosan quaternary ammonium salt was purchased from Shanghai Bide Pharmaceutical Technology Co., Ltd. (Article No.: BD02625758 Chitosanquaternary ammonium salt, 97%), and octadecyl hydroxypropyl sulfobetaine (DY-OHSB) was purchased from Shanghai Deyi Chemical Co., Ltd.;

[0030] Example 3: An environmentally friendly antibacterial composition, composed of the following mass percentages, lysozyme (CAS: 12650-88-3) 5%, dimethyl octadecyl [3- (trimethoxysilyl) propyl] ammonium chloride (CAS No.: 27668-52-6) 1%, octadecyl hydroxypropyl sulfobetaine (DY-OHSB) 3%, chitosan quaternary ammonium salt 2%, sodium alginate 2%, eugenol 1.5%, matrine 0.5%, PEG-60 hydrogenated castor oil 2%, 3-aminopropyl trimethoxysilane 1%, and the balance is deionized water; wherein chitosan quaternary ammonium salt was purchased from Shanghai Bide Pharmaceutical Technology Co., Ltd. (Article No.: BD02625758 Chitosan quaternaryammonium salt, 97%), and octadecyl hydroxypropyl sulfobetaine (DY-OHSB) was purchased from Shanghai Deyi Chemical Co., Ltd.;

[0031] Example 4: An environmentally friendly antibacterial composition, composed of the following mass percentages, lysozyme (CAS: 12650-88-3) 3%, dimethyl octadecyl [3- (trimethoxysilyl) propyl] ammonium chloride (CAS No.: 27668-52-6) 2%, octadecyl hydroxypropyl sulfobetaine (DY-OHSB) 2%, chitosan quaternary ammonium salt 4%, sodium alginate 1.5%, eugenol 1%, matrine 0.5%, PEG-60 hydrogenated castor oil 1.5%, 3-aminopropyl trimethoxysilane 0.5%, and the balance is deionized water; wherein chitosan quaternary ammonium salt was purchased from Shanghai Bide Pharmaceutical Technology Co., Ltd. (Article No.: BD02625758 Chitosanquaternary ammonium salt, 97%), and octadecyl hydroxypropyl sulfobetaine (DY-OHSB) was purchased from Shanghai Deyi Chemical Co., Ltd.;

[0032] Example 5: An environmentally friendly antibacterial composition, composed of the following mass percentages, lysozyme (CAS: 12650-88-3) 3%, dimethyl octadecyl [3-(trimethoxysilyl) propyl] ammonium chloride (CAS No.: 27668-52-6) 2%, octadecyl hydroxypropyl sulfobetaine (DY-OHSB) 2%, chitosan quaternary ammonium salt 3%, sodium alginate 2%, eugenol 1.5%, matrine 1%, PEG-60 hydrogenated castor oil 2%, 3-aminopropyl trimethoxysilane 1%, and the balance is deionized water; wherein chitosan quaternary ammonium salt was purchased from Shanghai Bide Pharmaceutical Technology Co., Ltd. (Article No.: BD02625758 Chitosan quaternaryammonium salt, 97%), and octadecyl hydroxypropyl sulfobetaine (DY-OHSB) was purchased from Shanghai Deyi Chemical Co., Ltd.;

[0033] Comparative Example 1 (without lysozyme): An environmentally friendly antibacterial composition, composed of the following mass percentages: 2% dimethyloctadecyl [3- (trimethoxysilyl) propyl] ammonium chloride (CAS No.: 27668-52-6), 2% octadecyl hydroxypropyl sulfobetaine (DY-OHSB), 3% chitosan quaternary ammonium salt, 2% sodium alginate, 1.5% eugenol, 1% matrine, 2% PEG-60 hydrogenated castor oil, 1% 3-aminopropyl trimethoxysilane, and the balance is deionized water; wherein chitosan quaternary ammonium salt was purchased from Shanghai Bide Pharmaceutical Technology Co., Ltd. (Article No.: BD02625758 Chitosan quaternary ammonium salt, 97%), and octadecyl hydroxypropyl sulfobetaine (DY-OHSB) was purchased from Shanghai Deyi Chemical Co., Ltd.;

[0034] Comparative Example 2 (without organic antibacterial agent): An environmentally friendly antibacterial composition, composed of the following mass percentages: lysozyme (CAS: 12650-88-3) 5%, sodium alginate 2%, eugenol 1.5%, matrine 0.5%, PEG-60 hydrogenated castor oil 2%, 3-aminopropyltrimethoxysilane 1%, and the balance deionized water;

[0035] Comparative Example 3 (without anti-mite agent): An environmentally friendly antibacterial composition, composed of the following mass percentages, lysozyme (CAS: 12650-88-3) 5%, dimethyl octadecyl [3-(trimethoxysilyl) propyl] ammonium chloride (CAS No.: 27668-52-6) 1%, octadecyl hydroxypropyl sulfobetaine (DY-OHSB) 3%, chitosan quaternary ammonium salt 2%, sodium alginate 2%, PEG-60 hydrogenated castor oil 2%, 3-aminopropyl trimethoxysilane 1%, and the balance is deionized water; wherein chitosan quaternary ammonium salt is purchased from Shanghai Bide Pharmaceutical Technology Co., Ltd. (Article No.: BD02625758 Chitosan quaternary ammonium salt, 97%), and octadecyl hydroxypropyl sulfobetaine (DY-OHSB) is purchased from Shanghai Deyi Chemical Co., Ltd.;

[0036] Comparative Example 4 (without stabilizer): An environmentally friendly antibacterial composition, composed of the following mass percentages, lysozyme (CAS: 12650-88-3) 3%, dimethyl octadecyl [3- (trimethoxysilyl) propyl] ammonium chloride (CAS No.: 27668-52-6) 1%, octadecyl hydroxypropyl sulfobetaine (DY-OHSB) 1%, chitosan quaternary ammonium salt 2%, PEG-60 hydrogenated castor oil 2%, eugenol 0.5%, matrine 0.5%, 3-aminopropyl trimethoxysilane 1%, and the balance is deionized water; wherein chitosan quaternary ammonium salt is purchased from Shanghai Bide Pharmaceutical Technology Co., Ltd. (Article No.: BD02625758 Chitosan quaternaryammonium salt, 97%), and octadecyl hydroxypropyl sulfobetaine (DY-OHSB) is purchased from Shanghai Deyi Chemical Co., Ltd.;

[0037] Comparative Example 5 (without coupling agent): An environmentally friendly antibacterial composition, composed of the following mass percentages, lysozyme (CAS: 12650-88-3) 5%, dimethyl octadecyl [3- (trimethoxysilyl) propyl] ammonium chloride (CAS No.: 27668-52-6) 1%, octadecyl hydroxypropyl sulfobetaine (DY-OHSB) 3%, chitosan quaternary ammonium salt 2%, sodium alginate 2%, eugenol 1.5%, matrine 0.5%, PEG-60 hydrogenated castor oil 2%, and the balance is deionized water; wherein chitosan quaternary ammonium salt is purchased from Shanghai Bide Pharmaceutical Technology Co., Ltd. (Article No.: BD02625758 Chitosan quaternary ammonium salt, 97%), and octadecyl hydroxypropyl sulfobetaine (DY-OHSB) is purchased from Shanghai Deyi Chemical Co., Ltd.;

[0038] The preparation methods of the environmentally friendly antibacterial compositions of Examples 1-5 and Comparative Examples 1-5 are as follows:

[0039] (1) Weighing the anti-mite agent, solubilizer and coupling agent according to mass percentage, adding deionized water, mixing and heating to 40-80° C., stirring evenly, and cooling to room temperature;

[0040] (2) weighing an organic antimicrobial agent according to mass percentage, adding it to step (1), and mixing and stirring uniformly;

[0041] (3) gradually adding the lysozyme solution into the stabilizer and mixing and stirring evenly;

[0042] (4) Mixing the enzyme mixed solution obtained in step (3) with the solution obtained in step (2), and adding the remaining amount of deionized water, and mixing them evenly to obtain an environmentally friendly antibacterial composition.

[0043] The preparation methods of the environmentally friendly antibacterial compositions of Comparative Examples 1-5 are the steps of reducing unnecessary raw materials in the preparation methods of Examples 1-5.

[0044] Example 6 Antimicrobial enzyme activity test of environmentally friendly antimicrobial composition

[0045] This method is based on the WS / T 647-2019 standard and evaluates the activity of lysozyme by measuring the hydrolysis of lysococcus substrate. Weigh 15 mg of lysococcus, add 0.5 mL to 1 mL of phosphate buffer, grind in a mortar for 3 minutes, and then add an appropriate amount of phosphate buffer to make the total volume about 50 mL. The absorbance of the suspension measured at 25℃±0.1℃ at a wavelength of 450nm is 0.70±0.05.

[0046] Take 3 mL of the substrate suspension at 25°C ± 0.1°C, place it in a colorimetric cell, measure the absorbance at a wavelength of 450 nm, and take 0.15 mL of the solution of Examples 1-5 and Comparative Examples 1-5 at 25°C ± 0.1°C, add it to the colorimetric cell, mix it quickly, use a stopwatch to time, and measure the absorbance A again at 60 seconds; at the same time, measure 0.15 mL of phosphate buffer, operate in the same way, as a blank test, and measure the reading A'0 at 0 seconds and the reading A' at 60 seconds.

[0047] Calculate the lysozyme activity in the sample to be tested, see the following formula:

[0048]

[0049] C--sample lysozyme activity (U / mL); N--dilution multiple.

[0050] Calculation of relative enzyme activity: Taking the enzyme activity of a single pure lysozyme solution as a reference, assuming the reference value to be 100%, the relative enzyme activity of the lysozyme in the compositions of Examples 1-5 and Comparative Examples 1-5 relative to the single pure lysozyme solution was calculated.

[0051] Table 1 Relative enzyme activity test results

[0052]

[0053]

[0054] The results in Table 1 show that, according to the relative enzyme activity test results, compared with the control group, the relative enzyme activity of the lysozymes in Examples 1-5 can be above 90%, indicating that the components in the composition have little effect on the enzyme activity; compared with Examples 1-5, no enzyme activity was detected in Comparative Example 1, the relative enzyme activity of the lysozymes in Comparative Examples 2, 3 and 5 can be above 90%, and the relative enzyme activity in Comparative Example 4 is less than 50%, which indicates that the stabilizer can protect the enzyme and reduce the damage of the system to the enzyme structure, thereby improving the enzyme activity stability of the enzyme in the system.

[0055] Example 7 Antibacterial Activity Test of Environmentally Friendly Antibacterial Composition

[0056] In order to quickly evaluate the antibacterial effects of the antibacterial compositions in Examples 1-5 and Comparative Examples 1-5, this experiment adopted a qualitative detection method, the Agar Diffusion Method, to evaluate the antibacterial effects of each composition by observing the size of the inhibition zone.

[0057] Escherichia coli, Staphylococcus aureus and Candida albicans were selected for antibacterial detection experiments. The bacterial strains to be tested were cultured in a suitable culture medium at 37°C for 24 hours. The cultured bacterial suspensions were diluted to 1×10 6CFU / mL, use a sterile cotton swab to dip the bacterial suspension and evenly apply it on the surface of the agar plate to ensure uniform bacterial growth on the surface of the plate. Take the antibacterial composition solution in Examples 1-5 and Comparative Examples 1-5, immerse the sterile filter paper in the antibacterial composition solution in Examples 1-5 and Comparative Examples 1-5, gently absorb the excess solution, and quickly place the filter paper on the surface of the agar plate inoculated with bacteria. Control group: replace the antibacterial composition solution with physiological saline. Set up at least three replicates for each antibacterial composition. Place the plate inoculated with the antibacterial composition in an incubator at 37°C and incubate for 24 hours. Observe and measure the diameter of the inhibition zone formed on the agar surface under the action of the antibacterial composition. The size of the inhibition zone is proportional to the antibacterial effect. The larger the inhibition zone, the stronger the antibacterial effect. Figure 1 .

[0058] Figure 1 The results showed that the antibacterial composition solutions of Examples 1-5 had antibacterial effects on Escherichia coli, Staphylococcus aureus and Candida albicans, respectively. In comparison, the antibacterial effect of the antibacterial composition solutions of Comparative Examples 1-4 was weaker and the inhibition zone was smaller. The antibacterial effect of the antibacterial composition solution of Comparative Example 5 was equivalent to that of the antibacterial composition of Examples 1-5. It can be seen that lysozyme, organic antibacterial agents and anti-mite agents can synergistically improve the antibacterial effect of the composition.

[0059] Example 8 Preparation of Cotton Fibers Coupled with Environmentally Friendly Antibacterial Compositions and Detection of Coupling Effects

[0060] Preparation method of antibacterial composition coupled cotton fiber:

[0061] Take an appropriate amount of cotton fiber, use deionized water and an appropriate amount of surfactant to clean it, remove surface grease, dirt and impurities, and ensure that the surface of the cotton fiber is clean. After cleaning, dry the cotton fiber in an oven at 60°C for 24 hours to ensure that there is no residual moisture. The antibacterial composition solution prepared according to the formula of Examples 1-5 and Comparative Examples 1-5 is diluted to a certain concentration to form a working solution, and then the pH of the solution is appropriately adjusted to 4-6 using dilute hydrochloric acid to promote the hydrolysis reaction of silane. Soak the cleaned cotton fiber in the prepared working solution to ensure that the fiber surface is evenly contacted with the solution. The soaking time is 30 minutes to 2 hours. The solution can be gently stirred to ensure that the composition can fully penetrate the fiber surface, and the reaction system is heated to 40-60°C, but the temperature should not be too high to avoid damage to the cotton fiber and lysozyme. The treated cotton fiber is placed in an oven at 40-60°C for heat treatment for 30 minutes to 1 hour. This process helps to promote further bonding of the silane coupling agent with the surface of the cotton fiber and increase the stability of the fiber surface coating. The treated cotton fiber is naturally air-dried to ensure the uniformity and stability of the antibacterial coating, thereby obtaining the antibacterial cotton fiber samples of Examples 1-5 and Comparative Examples 1-5.

[0062] XPS binding strength analysis of antibacterial cotton fiber samples:

[0063] The antibacterial cotton fiber samples of Examples 1-5, Comparative Examples 4-5, and the cotton fiber samples modified with silane alone were dried (vacuum dried at 40°C for 24h) to avoid moisture affecting the surface chemical analysis, and fixed on the XPS sample holder to ensure uniform exposure of the fiber surface. An Al Kα X-ray source (1486.6eV) was used, and the working pressure was <10 -8 Pa. Collect the Si2p spectrum (100-105eV), and focus on analyzing the Si-O-Cellulose characteristic peak (102.5eV) and silicon oxide (103-104eV). If the 102.5eV characteristic peak is detected, it means that the silane coupling agent successfully forms a Si-O-Cellulose bond on the fiber surface, and the binding force is strong. If the characteristic peak shifts or disappears, it means that the silane coupling agent is not effectively bound or the binding force is weak.

[0064] Analysis of antibacterial cotton fiber sample washability:

[0065] Take the antibacterial cotton fiber samples of Examples 1-5, Comparative Examples 1-5, and the cotton fiber samples modified with silane only, and wash them 100 times (according to ISO 6330 standard). XPS analysis is performed after each washing to monitor the changes in the Si-O-Cellulose characteristic peak. If the 102.5eV peak intensity decreases significantly, it means that the binding force is weak; if the peak remains stable, it indicates that the binding is strong.

[0066] Table 2 XPS binding analysis

[0067]

[0068] The XPS test in Table 2 shows that the antibacterial cotton of Examples 1-5 successfully forms Si-O-Cellulose bonds at 102.5 eV; compared with the antibacterial cotton of Comparative Example 4, the antibacterial cotton of Examples 1-5 has strong binding force, is resistant to water washing, and has excellent stability.

[0069] Characterization of lysozyme by fluorescence labeling to analyze the cross-linking effect of antibacterial cotton fiber samples:

[0070] Lysozyme was labeled with fluorescein isothiocyanate (FITC, green fluorescence) to prepare an environmentally friendly antibacterial composition with lysozyme labeled with green fluorescence (FITC-lysozyme). The fabric was treated with a post-finishing process under a light-proof environment, and then the distribution of green fluorescent protein on the cotton fabric was observed by laser confocal microscopy to observe the presence of lysozyme on the cotton fabric and characterize the successful attachment of lysozyme to the cotton fabric. Experimental group: antibacterial cotton fiber sample of Example 1; control group: antibacterial cotton fiber sample of Comparative Example 1, see Figure 2 .

[0071] Figure 2 The results showed that compared with the cotton fibers in the control group (comparative example 1 without lysozyme treatment), the cotton fibers in the experimental group (lysozyme treatment in example 1) were distributed with green fluorescent protein, indicating that lysozyme was successfully fixed on the cotton fiber fabric.

[0072] Example 9 Antibacterial effect test and anti-mite effect test of antibacterial cotton based on environmentally friendly antibacterial composition

[0073] The antibacterial cotton fiber samples of Examples 1-5 and Comparative Examples 1-5 prepared in Example 8 were evaluated for antibacterial properties according to GB / T20944.3-2008 "Evaluation of antibacterial properties of textiles Part 3: Oscillation method" and T / SZTIA001-2023 "Antibacterial textiles" standards. The antibacterial rate results are shown in Table 3.

[0074] Table 3 Evaluation of antibacterial properties of antibacterial cotton cloth

[0075]

[0076] The results in Table 3 show that the antibacterial cotton cloths of Examples 1-5 have good antibacterial effects on Escherichia coli, Staphylococcus aureus and Candida albicans. The initial antibacterial effect is basically > 99% for the three bacteria, and after washing 150 times, it can still reach T / SZTIA. The 7A antibacterial level specified in the 001-2023 "Antibacterial Textiles" standard indicates that the antibacterial cotton cloth has good water washing resistance, the environmentally friendly antibacterial composition of the present invention is tightly combined with the fabric, and the antibacterial cotton fabric has long-lasting antibacterial properties; while the antibacterial cotton fabrics prepared in comparative examples 1-5 do not contain antibacterial enzymes or organic antibacterial agents or anti-mite agents or stabilizers or coupling agents, and their antibacterial effects are lower than those of examples 1-5, which shows that the antibacterial enzymes and organic antibacterial agents can play a synergistic role and improve the overall antibacterial effect of the cotton fabric; the stabilizer can effectively improve the stability of the enzyme activity and ensure that the enzyme exerts its antibacterial effect; the coupling agent can increase the loading rate of the antibacterial composition on the fabric and the water washing resistance of the antibacterial fabric, thereby achieving the long-lasting antibacterial effect of the antibacterial cotton fabric.

[0077] Fabric anti-mite effect test:

[0078] The antibacterial cotton fiber samples of Examples 1-5 and Comparative Examples 1-3 prepared in Example 8 were evaluated for their anti-mite performance according to GB / T24253-2009 “Evaluation of Anti-mite Performance of Textiles”. The mite repellency results are shown in Table 4.

[0079] Table 4 Evaluation of antibacterial cotton cloth's anti-mite performance

[0080] Group Action time Average number of mites Repellency rate (%) Control group 24h 264 / Example 1 24h 42 82 Example 2 24h 45 83 Example 3 24h 34 87 Example 4 24h 35 86 Example 5 24h 43 85 Comparative Example 1 24h 102 75 Comparative Example 2 24h 103 53 Comparative Example 3 24h 158 43

[0081] The results in Table 4 show that the antibacterial cotton fabrics of Examples 1-5 have a mite repellency rate of ≥80%, which have a strong anti-mite effect. However, the antibacterial cotton fabrics prepared in Comparative Examples 1-3 without antibacterial enzymes, organic antibacterial agents or anti-mite agents have a mite repellency rate lower than that of Examples 1-5, indicating that lysozyme, organic antibacterial agents and anti-mite agents can synergistically improve the anti-mite effect of the composition.

[0082] The above is a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. An environmentally friendly antibacterial composition, characterized in that: The environmentally friendly antibacterial composition comprises an antibacterial enzyme, a stabilizer, an organic antibacterial agent, an anti-mite agent, a solubilizer and a coupling agent, including the following mass percentages: 0.2%-20% of antibacterial enzyme, 2%-30% of organic antibacterial agent, 0.5%-10% of stabilizer, 0.5%-10% of anti-mite agent, 1%-20% of solubilizer, 0.5%-5% of coupling agent, and the balance is deionized water.

2. The environmentally friendly antibacterial composition according to claim 1, wherein the antibacterial enzyme comprises any one of lysostaphin, subtilisin, bacteriophage lytic enzyme, lysozyme, alginate lyase, glucose oxidase, cellobiose dehydrogenase, lactoperoxidase, and myeloperoxidase, or a combination thereof.

3. The environmentally friendly antibacterial composition according to claim 1, wherein the stabilizer comprises one or a combination of alginic acid, alginate, sodium dextran phosphate, gelatin, xanthan gum, sodium polyacrylate, polyacrylate, polyvinyl alcohol, polyvinyl pyrrolidone, polybetaine, vinylimidazole polymer, and polyethyleneimine.

4. The environmentally friendly antibacterial composition according to claim 1, wherein the organic antibacterial agent comprises a synthetic organic antibacterial agent, a natural or naturally modified organic antibacterial agent, or a combination thereof; further, the synthetic organic antibacterial agent comprises a guanidine salt, a quaternary ammonium salt, and a betaine antibacterial agent, or a combination thereof; further, the synthetic organic antibacterial agent comprises polyhexamethylene guanidine hydrochloride (PHMG), polyhexamethylene biguanide hydrochloride (PHMB), dodecyl trimethyl ammonium chloride, dioctadecyl dimethyl ammonium chloride, dimethyl octadecyl [3- (trimethoxysilyl) propyl] ammonium chloride, tetrapyridine chloride, benzethonium chloride, cocamidopropyl betaine, octadecyl propyl betaine, (C 12 ~C 18 ) one or a combination of alkyl sulfopropyl betaine and octadecyl hydroxypropyl sulfobetaine; the natural or naturally modified organic antibacterial agent includes one or a combination of lignin, chitin, fucoidan, antimicrobial peptides, chitosan, hydroxylated chitosan, carboxymethyl chitosan, acylated chitosan, N-trimethyl chitosan, chitosan hydrochloride, chitosan quaternary ammonium salt and chitosan sulfate.

5. The environmentally friendly antibacterial composition according to claim 1, wherein the anti-mite agent is a plant extract, including one or a combination of eugenol, eucalyptus leaf extract, tea tree oil, matrine, geraniol, lavender oil, and cinnamon oil.

6. The environmentally friendly antibacterial composition according to claim 1, wherein the solubilizer comprises one or a combination of PEG-60 hydrogenated castor oil, polyglyceryl-2 triisostearate, propylene glycol, hexylene glycol, isohexylene glycol, caprylyl glycol and polyethylene glycol.

7. The environmentally friendly antibacterial composition according to claim 1, wherein the coupling agent is one or a combination of vinyl silane, aminosilane, epoxysilane, and mercaptosilane, and further comprises one or a combination of vinyltrimethoxysilane, 3-aminopropyltrimethoxysilane, γ-mercaptopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, and γ-(3,2-epoxypropoxy)methyltrimethoxysilane.

8. A cotton fabric comprising the environmentally friendly antibacterial composition according to any one of claims 1 to 7, characterized in that: The cotton fabric has excellent antibacterial and anti-mite performance, with an antibacterial rate of more than 99%, and after being washed 150 times, it can still reach the 7A antibacterial level, and the mite repellent rate is more than or equal to 80%.

9. Use of the environmentally friendly antibacterial composition according to any one of claims 1 to 7 in the preparation of antibacterial and anti-mite textiles.

10. A method for preparing an antibacterial textile, characterized in that: The preparation method comprises the following steps: taking a textile and the environmentally friendly antibacterial composition according to any one of claims 1 to 7; soaking the textile with the environmentally friendly antibacterial composition for textiles, uniformly cross-linking the textile, and then drying the textile.

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