Preparation method and application of biological functional agent containing bioactive components
By using zeolite-loaded titanium dioxide composite material and compounding technology of mint leaves and aloe vera powder, biological functional agents were prepared, which solved the problem of insufficient stability and loading of biological active ingredients, and achieved efficient sustained release and antibacterial effects.
Patent Information
- Application Number
- CN202411567909.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-05
- Publication Date
- 2025-02-14
- Estimated Expiration
- 2044-11-05
AI Technical Summary
During the preparation of biological functional agents, the stability and loading of the biologically active ingredients are insufficient, resulting in poor sustained release effect, affecting its application range and efficiency.
Using zeolite-loaded titanium dioxide composite material as a carrier, combined with the combination technology of mint leaves and aloe powder, a mixed solution containing biological active ingredients was prepared through ultrasonic extraction and rotary evaporation, and a biological functional agent was obtained by stirring and centrifugation. .
It improves the loading and stability of the biologically active ingredients, enhances the sustained release effect, and significantly improves the antibacterial properties and application range of biological functional agents.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of biofunctional agents, and in particular to a method for preparing a biofunctional agent containing bioactive components. Background Art
[0002] In the context of modern scientific and technological development, the preparation and application of biofunctional agents have gradually become a research hotspot. Such functional agents are widely used in many fields such as medicine, environmental protection, and materials science because of their specific bioactive ingredients. Biofunctional agents are usually prepared by extracting and purifying bioactive ingredients existing in nature. These bioactive ingredients have multiple functions such as antiviral, antibacterial, and antioxidant. Therefore, it is of great significance to develop functional agents containing these ingredients.
[0003] During the preparation process, the required bioactive ingredients must first be extracted from plants, microorganisms or animals. This step usually involves a variety of chemical and physical methods, such as solvent extraction, ultrasonic extraction, microwave extraction, etc., to ensure efficient and complete extraction of the target ingredients. After the extraction is completed, the next step is the purification process of the bioactive ingredients. Purification is to remove impurities in the extract and improve the purity and stability of the bioactive ingredients. Common purification methods include crystallization, chromatography, membrane separation, etc. Through purification, bioactive ingredients with higher purity can be obtained, laying a good foundation for the subsequent preparation of functional agents.
[0004] When preparing biofunctional agents, it is usually necessary to compound the purified bioactive ingredients with other substances to improve their stability and application range. For example, bioactive ingredients can be compounded with polymers, inorganic materials, etc. to form functional agents with specific properties. In addition, molecular capsules, molecular nests and other technologies can be used to embed and protect bioactive ingredients to improve their stability and bioavailability.
[0005] In recent years, with the continuous development of nanotechnology and biotechnology, more and more new technologies have been applied to the preparation of biofunctional agents. For example, nanotechnology can be used to prepare bioactive ingredients into nanoparticles to improve their solubility and biological activity; biotechnology can be used to construct microbial communities with specific functions to prepare biofunctional agents with special properties.
[0006] In terms of specific applications, biofunctional agents containing bioactive ingredients have broad application prospects in the medical field. For example, drugs with antiviral and antibacterial functions can be prepared; in the field of environmental protection, biofunctional agents for degrading organic pollutants can be prepared; in the field of materials science, biocomposite materials with special properties can be prepared. Based on this, the present invention provides a method for preparing a biofunctional agent containing bioactive ingredients. Summary of the invention
[0007] The purpose of the present invention is to provide a method for preparing a biofunctional agent containing a bioactive component, thereby increasing the loading amount of the bioactive component on a carrier, improving the stability of the bioactive component, and enhancing the sustained-release effect.
[0008] On the one hand, the present invention provides a method for preparing a biofunctional agent containing bioactive ingredients, the steps comprising: dispersing the bioactive ingredients in water, adding zeolite-loaded titanium dioxide composite material, anhydrous ethanol, isopropyl triisostearyl titanate and polyvinyl pyrrolidone thereto, stirring at a temperature of 65-75°C to obtain a mixed solution containing the bioactive ingredients, stirring for 80-100 minutes and then centrifuging and drying to obtain the mixed solution.
[0009] Furthermore, the weight ratio of the bioactive ingredient, water, zeolite-supported titanium dioxide composite material, anhydrous ethanol, triisostearyl isopropyl titanate and polyvinyl pyrrolidone is (20-22):
[0010] (60-80):(3-5):(30-40):(6-8):(5-7).
[0011] Furthermore, the preparation method of the bioactive ingredient includes: washing and drying mint leaves and aloe vera with a water content of less than 5%, respectively crushing them through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, then mixing them evenly to obtain a mixed powder, taking the mixed powder and adding it into ethanol for ultrasonication for 40-60 minutes, filtering and concentrating the filtrate by rotary evaporation to 30-34% of the volume of the filtrate, and then centrifuging the concentrated solution to obtain the bioactive ingredient.
[0012] Furthermore, the cleaning method includes rinsing with a NaOH solution having a mass concentration of 10-12% for 4-6 times, and then immersing and washing with deionized water for 2-4 times, with the immersion time being 20-30 seconds.
[0013] Furthermore, the usage ratio of the mint leaf powder, aloe powder and ethanol is (20-22) g: (12-13) g: (190-210) mL.
[0014] Furthermore, the preparation method of the zeolite-loaded titanium dioxide composite material includes: adding zeolite to ethanol for ultrasonic dispersion for 30-40 minutes, adding tetrabutyl titanate at a speed of 200-300 r / min, then adding a Na2CO3 solution with a mass concentration of 4-6%, condensing and refluxing, centrifuging, washing and drying.
[0015] Furthermore, the usage ratio of the zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution is (60-80) mg: (60-80) mL: (0.02-0.04) g: (1.4-1.6) mL.
[0016] Furthermore, the condensation reflux temperature is 82-86° C. and the time is 8-10 h.
[0017] On the other hand, the present invention also provides a method for preparing a biofunctional agent containing a bioactive component and application of the prepared biofunctional agent in antibacterial products.
[0018] Furthermore, the antimicrobial product includes textiles, fibers or coatings.
[0019] The beneficial effects of the present invention are:
[0020] (1) The bioactive ingredients in the present invention include mint leaves and aloe vera powder. Both plants are rich in bioactive ingredients, such as menthol and aloe polysaccharides, and have extensive medical and health values. When the two are compounded, the alcohols, ketones and other ingredients in the mint leaves form hydrogen bonds with the polysaccharides, organic acids and other ingredients in the aloe vera powder, which can stabilize the structure of the compound and prevent mutual collision and decomposition between molecules. At the same time, they may also protect each other through steric hindrance effects, making the entire compound system more stable, which is conducive to the preservation and release of bioactive ingredients.
[0021] (2) The extraction method of the biologically active components of the aloe powder in the present invention is simple, and is a direct drying and crushing method. It has a certain water absorption capacity, and can improve the air permeability of the material when combined with the mint active component, which is mainly due to the porous structure of the aloe powder and the volatility of the mint component. The porous structure of the aloe powder gives it good air permeability, allowing air and water molecules to pass freely; in addition, the aloe active components can also have high temperature resistance to a certain extent, which is mainly related to its chemical structure and stability; the biologically active components such as polysaccharides and anthraquinone compounds in aloe have high thermal stability and can maintain their structure and activity under certain high temperature conditions;
[0022] (3) After the biological functional agent prepared in the present invention is used to prepare polyester fiber, it has a high inhibition rate against Staphylococcus aureus, Escherichia coli, Klebsiella pneumoniae and Candida albicans; the menthol, menthone and other components in mint leaves and the polysaccharides and anthraquinone compounds in aloe vera have significant antibacterial activity. These components can destroy the cell wall or cell membrane of bacteria and inhibit their growth and reproduction; the interaction between the two after mixing can enhance the antibacterial effect of each other;
[0023] (4) The present invention uses a zeolite-loaded titanium dioxide composite material as a carrier to load biologically active ingredients, which has a controlled sustained release property. Furthermore, when washed with high-temperature water, the active sites can still adsorb and fix the aloe active ingredients, making it difficult for them to be washed away by water. In addition, when mint leaves and aloe powder are compounded, the active ingredients in the mint powder interact with the active sites on the surface of the zeolite-loaded titanium dioxide composite material, thereby increasing the number of active sites on the surface of the composite material. These increased active sites can more effectively adsorb and fix the aloe active ingredients and enhance the binding force between the two. Therefore, the functional polyester fiber prepared using the biological functional agent can still maintain a good bactericidal effect after washing with water at 50°C.
[0024] (5) When zeolite-loaded titanium dioxide composite materials are used as carriers, the porous structure of zeolite is utilized. These micropores and mesopores are like tiny "storage rooms", providing abundant adsorption sites for bioactive ingredients. By introducing titanium dioxide, not only the surface properties of zeolite are optimized, but also the interaction between zeolite and bioactive ingredients is enhanced, thereby greatly increasing the loading amount of bioactive ingredients on the composite material. This means that more bioactive ingredients can be carried per unit mass of the composite material, improving the overall efficiency of the material; the combination of the porous structure of zeolite and the coating effect of titanium dioxide provides a fine regulation mechanism for the release of bioactive ingredients, achieving slow and continuous release of bioactive ingredients. This sustained-release characteristic not only prolongs the action time of the bioactive ingredients, but also improves the utilization rate of the bioactive ingredients;
[0025] (6) The biofunctional agent prepared in the present invention has excellent sustained-release performance and bactericidal performance, and its application level can also be expanded to products such as textiles, masks and coatings. DETAILED DESCRIPTION
[0026] The technical scheme of the present invention is described clearly and completely below. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in the field without creative work are within the scope of protection of the present invention. Raw materials not specified in the following embodiments are all commercially available.
[0027] Example 1
[0028] This embodiment provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0029] (1) Preparation of biologically active ingredients: Mint leaves and aloe vera that have been washed and dried to a water content of less than 5% are crushed through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, respectively, and then mixed to obtain a mixed powder. The mixed powder is added to ethanol and ultrasonicated for 50 minutes. After filtering, the filtrate is concentrated by rotary evaporation to 32% of the volume of the filtrate, and then the concentrated solution is centrifuged to obtain the biologically active ingredient; the washing method includes rinsing with a NaOH solution with a mass concentration of 11% for 5 times, and then immersing and washing with deionized water for 3 times, and the immersion time is 25 seconds; the amount ratio of mint leaf powder, aloe vera powder and ethanol is 21g:12.5g:200mL;
[0030] (2) Preparation of zeolite-loaded titanium dioxide composite material: zeolite was added to ethanol and ultrasonically dispersed for 35 min, tetrabutyl titanate was added at a speed of 250 r / min, and then a 5% mass concentration of Na2CO3 solution was added and condensed and refluxed at a temperature of 84°C for 9 h, centrifuged, washed and dried to obtain the composite material; the dosage ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution was 70 mg: 70 mL: 0.03 g: 1.5 mL;
[0031] (3) Preparation of biofunctional agent: The bioactive component is dispersed in water, and zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone are added thereto and stirred at 70°C to obtain a mixed solution containing the bioactive component. The mixed solution is stirred for 90 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone is 21:70:4:35:7:6.
[0032] Example 2
[0033] This embodiment provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0034] (1) Preparation of biologically active ingredients: mint leaves and aloe vera that have been washed and dried to a water content of less than 5% are crushed through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, and then mixed to obtain a mixed powder. The mixed powder is added to ethanol and ultrasonicated for 40 minutes. After filtering, the filtrate is concentrated by rotary evaporation to 30% of the volume of the filtrate, and then the concentrated solution is centrifuged to obtain the biologically active ingredient; the washing method includes rinsing with a 10% NaOH solution for 4 times, and then immersing and washing with deionized water for 2 times, and the immersion time is 20 seconds; the amount ratio of mint leaf powder, aloe vera powder and ethanol is 20g:12g:190mL;
[0035] (2) Preparation of zeolite-loaded titanium dioxide composite material: zeolite was added to ethanol and ultrasonically dispersed for 30 min, tetrabutyl titanate was added at a speed of 200 r / min, and then a 4% Na2CO3 solution was added and condensed and refluxed at a temperature of 82°C for 8 h, centrifuged, washed and dried to obtain the composite material; the dosage ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution was 60 mg: 60 mL: 0.02 g: 1.4 mL;
[0036] (3) Preparation of biofunctional agents: The bioactive ingredients are dispersed in water, and zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone are added thereto and stirred at 65°C to obtain a mixed solution containing the bioactive ingredients. The mixed solution is stirred for 80 minutes and then centrifuged and dried. The weight ratio of the bioactive ingredients, water, zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone is 20:60:3:30:6:5.
[0037] Example 3
[0038] This embodiment provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0039] (1) Preparation of biologically active ingredients: mint leaves and aloe vera that have been washed and dried to a water content of less than 5% are crushed through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, respectively, and then mixed to obtain a mixed powder. The mixed powder is added to ethanol and ultrasonicated for 60 minutes. After filtering, the filtrate is concentrated by rotary evaporation to 34% of the filtrate volume, and then the concentrated solution is centrifuged to obtain the biologically active ingredient; the washing method includes rinsing with a 12% NaOH solution for 6 times, and then immersing and washing with deionized water for 4 times, and the immersion time is 30 seconds; the amount ratio of mint leaf powder, aloe vera powder and ethanol is 22g:13g:210mL;
[0040] (2) Preparation of zeolite-loaded titanium dioxide composite material: zeolite was added to ethanol and ultrasonically dispersed for 40 min, tetrabutyl titanate was added at a speed of 300 r / min, and then a Na2CO3 solution with a mass concentration of 6% was added and condensed and refluxed at a temperature of 86°C for 10 h, and the mixture was centrifuged, washed and dried. The amount ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution was 80 mg: 80 mL: 0.04 g: 1.6 mL.
[0041] (3) Preparation of biofunctional agent: The bioactive component is dispersed in water, and zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone are added thereto and stirred at 75°C to obtain a mixed solution containing the bioactive component. The solution is stirred for 100 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone is 22:80:5:40:8:7.
[0042] Example 4
[0043] This embodiment provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0044] (1) Preparation of biologically active ingredients: mint leaves and aloe vera that have been washed and dried to a water content of less than 5% are crushed through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, respectively, and then mixed to obtain a mixed powder. The mixed powder is added to ethanol and ultrasonicated for 40 minutes. After filtering, the filtrate is concentrated by rotary evaporation to 34% of the filtrate volume, and then the concentrated solution is centrifuged to obtain the bioactive ingredient; the washing method includes rinsing with a 10% NaOH solution for 6 times, and then immersing and washing with deionized water for 2 times, and the immersion time is 30 seconds; the amount ratio of mint leaf powder, aloe vera powder and ethanol is 20g:13g:190mL;
[0045] (2) Preparation of zeolite-loaded titanium dioxide composite material: zeolite was added to ethanol and ultrasonically dispersed for 40 min, tetrabutyl titanate was added at a speed of 200 r / min, and then a Na2CO3 solution with a mass concentration of 6% was added and condensed and refluxed at a temperature of 82°C for 10 h, and the mixture was centrifuged, washed and dried. The amount ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution was 60 mg: 80 mL: 0.02 g: 1.6 mL.
[0046] (3) Preparation of biofunctional agent: The bioactive component is dispersed in water, and zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone are added thereto and stirred at 65°C to obtain a mixed solution containing the bioactive component. The solution is stirred for 100 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone is 20:80:3:40:6:7.
[0047] Comparative Example 1
[0048] This comparative example provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0049] (1) Preparation of biologically active ingredients: Aloe vera that has been washed and dried to a water content of less than 5% is crushed through a 60-mesh sieve to obtain aloe vera powder, the powder is added to ethanol and ultrasonicated for 50 minutes, the filtrate is filtered and concentrated by rotary evaporation to 32% of the filtrate volume, and the concentrated solution is then centrifuged to obtain the biologically active ingredient; the washing method includes rinsing with a NaOH solution with a mass concentration of 11% for 5 times, and then immersing and washing with deionized water for 3 times, the immersion time being 25 seconds; the amount ratio of aloe vera powder to ethanol is 33.5 g:200 mL;
[0050] (2) Preparation of zeolite-loaded titanium dioxide composite material: zeolite was added to ethanol and ultrasonically dispersed for 35 min, tetrabutyl titanate was added at a speed of 250 r / min, and then a 5% mass concentration of Na2CO3 solution was added and condensed and refluxed at a temperature of 84°C for 9 h, centrifuged, washed and dried to obtain the composite material; the dosage ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution was 70 mg: 70 mL: 0.03 g: 1.5 mL;
[0051] (3) Preparation of biofunctional agent: The bioactive component is dispersed in water, and zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone are added thereto and stirred at 70°C to obtain a mixed solution containing the bioactive component. The mixed solution is stirred for 90 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone is 21:70:4:35:7:6.
[0052] Comparative Example 2
[0053] This comparative example provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0054] (1) Preparation of bioactive ingredients: Wash and dry mint leaves with a water content of less than 5% and crush them through a 60-mesh sieve to obtain mint leaf powder, then add them into ethanol and perform ultrasonic treatment for 50 minutes, filter and concentrate the filtrate by rotary evaporation to 32% of the filtrate volume, then centrifuge the concentrated solution to obtain mint leaf extract, and then mix it with aloe extract powder purchased from Weiyi Peptide (Guangdong) Biotechnology Co., Ltd., wherein the ratio of mint leaf extract to aloe extract is 21:12.5; the washing method includes rinsing with a NaOH solution with a mass concentration of 11% for 5 times, and then immersing and washing with deionized water for 3 times, and the immersion time is 25 seconds; the amount ratio of mint leaf powder to ethanol is 33.5g:200mL;
[0055] (2) Preparation of zeolite-loaded titanium dioxide composite material: zeolite was added to ethanol and ultrasonically dispersed for 35 min, tetrabutyl titanate was added at a speed of 250 r / min, and then a 5% mass concentration of Na2CO3 solution was added and condensed and refluxed at a temperature of 84°C for 9 h, centrifuged, washed and dried to obtain the composite material; the dosage ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution was 70 mg: 70 mL: 0.03 g: 1.5 mL;
[0056] (3) Preparation of biofunctional agent: The bioactive component is dispersed in water, and zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone are added thereto and stirred at 70°C to obtain a mixed solution containing the bioactive component. The mixed solution is stirred for 90 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone is 21:70:4:35:7:6.
[0057] Comparative Example 3
[0058] This comparative example provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0059] (1) Preparation of bioactive ingredients: Wash and dry mint leaves to a water content of less than 5% and crush them through a 60-mesh sieve to obtain mint leaf powder. The powder is added to ethanol and ultrasonicated for 50 minutes. After filtering, the filtrate is concentrated by rotary evaporation to 32% of the filtrate volume, and then the concentrated solution is centrifuged to obtain the bioactive ingredient; the washing method includes washing with a NaOH solution with a mass concentration of 11% for 5 times, and then immersing and washing with deionized water for 3 times, and the immersion time is 25 seconds; the amount ratio of mint leaf powder to ethanol is 33.5g:200mL;
[0060] (2) Preparation of zeolite-loaded titanium dioxide composite material: zeolite was added to ethanol and ultrasonically dispersed for 35 min, tetrabutyl titanate was added at a speed of 250 r / min, and then a 5% mass concentration of Na2CO3 solution was added and condensed and refluxed at a temperature of 84°C for 9 h, centrifuged, washed and dried to obtain the composite material; the dosage ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution was 70 mg: 70 mL: 0.03 g: 1.5 mL;
[0061] (3) Preparation of biofunctional agent: The bioactive component is dispersed in water, and zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone are added thereto and stirred at 70°C to obtain a mixed solution containing the bioactive component. The mixed solution is stirred for 90 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone is 21:70:4:35:7:6.
[0062] Comparative Example 4
[0063] This comparative example provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0064] (1) Preparation of biologically active ingredients: Wash and dry mugwort and aloe vera to a water content of less than 5%, respectively, and grind them through a 60-mesh sieve to obtain mugwort powder and aloe vera powder, then mix them evenly to obtain a mixed powder, take the mixed powder and add it into ethanol for ultrasonic treatment for 50 minutes, filter and concentrate the filtrate by rotary evaporation to 32% of the volume of the filtrate, and then centrifuge the concentrated solution to obtain the biologically active ingredients; the washing method includes rinsing with a NaOH solution with a mass concentration of 11% for 5 times, and then immersing and washing with deionized water for 3 times, and the immersion time is 25 seconds; the amount ratio of mugwort powder, aloe vera powder and ethanol is 21g:12.5g:200mL;
[0065] (2) Preparation of zeolite-loaded titanium dioxide composite material: zeolite was added to ethanol and ultrasonically dispersed for 35 min, tetrabutyl titanate was added at a speed of 250 r / min, and then a 5% mass concentration of Na2CO3 solution was added and condensed and refluxed at a temperature of 84°C for 9 h, centrifuged, washed and dried to obtain the composite material; the dosage ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution was 70 mg: 70 mL: 0.03 g: 1.5 mL;
[0066] (3) Preparation of biofunctional agent: The bioactive component is dispersed in water, and zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone are added thereto and stirred at 70°C to obtain a mixed solution containing the bioactive component. The mixed solution is stirred for 90 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone is 21:70:4:35:7:6.
[0067] Comparative Example 5
[0068] This comparative example provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0069] (1) Preparation of biologically active ingredients: Mint leaves and aloe vera that have been washed and dried to a water content of less than 5% are crushed through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, respectively, and then mixed to obtain a mixed powder. The mixed powder is added to ethanol and ultrasonicated for 50 minutes. After filtering, the filtrate is concentrated by rotary evaporation to 32% of the volume of the filtrate, and then the concentrated solution is centrifuged to obtain the biologically active ingredient; the washing method includes rinsing with a NaOH solution with a mass concentration of 11% for 5 times, and then immersing and washing with deionized water for 3 times, and the immersion time is 25 seconds; the amount ratio of mint leaf powder, aloe vera powder and ethanol is 21g:12.5g:200mL;
[0070] (2) Preparation of biofunctional agent: The bioactive component is dispersed in water, and zeolite, anhydrous ethanol, isopropyl triisostearoyl titanate and polyvinyl pyrrolidone are added thereto and stirred at 70°C to obtain a mixed solution containing the bioactive component. The solution is stirred for 90 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, zeolite, anhydrous ethanol, isopropyl triisostearoyl titanate and polyvinyl pyrrolidone is 21:70:4:35:7:6.
[0071] Comparative Example 6
[0072] This comparative example provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0073] (1) Preparation of biologically active ingredients: Mint leaves and aloe vera that have been washed and dried to a water content of less than 5% are crushed through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, respectively, and then mixed to obtain a mixed powder. The mixed powder is added to ethanol and ultrasonicated for 50 minutes. After filtering, the filtrate is concentrated by rotary evaporation to 32% of the volume of the filtrate, and then the concentrated solution is centrifuged to obtain the biologically active ingredient; the washing method includes rinsing with a NaOH solution with a mass concentration of 11% for 5 times, and then immersing and washing with deionized water for 3 times, and the immersion time is 25 seconds; the amount ratio of mint leaf powder, aloe vera powder and ethanol is 21g:12.5g:200mL;
[0074] (2) Preparation of zeolite-loaded silica composite material: zeolite was added to ethanol and ultrasonically dispersed for 35 min, tetraethyl orthosilicate was added at a speed of 250 r / min, and then ammonia water was added to adjust the pH to 8-12, magnetically stirred for 2-7 h at room temperature in a closed state, centrifuged, washed and dried to obtain the composite material; the dosage ratio of zeolite, ethanol and tetraethyl orthosilicate was 70 mg: 140 mL: 0.03 g;
[0075] (3) Preparation of biofunctional agent: The bioactive component is dispersed in water, and zeolite-loaded silica composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone are added thereto and stirred at 70°C to obtain a mixed solution containing the bioactive component. The mixed solution is stirred for 90 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, zeolite-loaded silica composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone is 21:70:4:35:7:6.
[0076] Comparative Example 7
[0077] This comparative example provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0078] (1) Preparation of biologically active ingredients: Mint leaves and aloe vera that have been washed and dried to a water content of less than 5% are crushed through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, respectively, and then mixed to obtain a mixed powder. The mixed powder is added to ethanol and ultrasonicated for 50 minutes. After filtering, the filtrate is concentrated by rotary evaporation to 32% of the volume of the filtrate, and then the concentrated solution is centrifuged to obtain the biologically active ingredient; the washing method includes rinsing with a NaOH solution with a mass concentration of 11% for 5 times, and then immersing and washing with deionized water for 3 times, and the immersion time is 25 seconds; the amount ratio of mint leaf powder, aloe vera powder and ethanol is 21g:12.5g:200mL;
[0079] (2) Preparation of silica-supported titanium dioxide composite material: zeolite was added to ethanol and ultrasonically dispersed for 35 min, tetrabutyl titanate was added at a speed of 250 r / min, and then a 5% Na2CO3 solution was added and condensed and refluxed at a temperature of 84°C for 9 h, centrifuged, washed and dried to obtain the composite material; the dosage ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution was 70 mg: 70 mL: 0.03 g: 1.5 mL;
[0080] (3) Preparation of biofunctional agent: The bioactive component is dispersed in water, and silica-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone are added thereto and stirred at 70°C to obtain a mixed solution containing the bioactive component. The solution is stirred for 90 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, silica-loaded titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl and polyvinyl pyrrolidone is 21:70:4:35:7:6.
[0081] Comparative Example 8
[0082] This comparative example provides a method for preparing a biofunctional agent containing a bioactive component, the steps comprising:
[0083] (1) Preparation of biologically active ingredients: Mint leaves and aloe vera that have been washed and dried to a water content of less than 5% are crushed through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, respectively, and then mixed to obtain a mixed powder. The mixed powder is added to ethanol and ultrasonicated for 50 minutes. After filtering, the filtrate is concentrated by rotary evaporation to 32% of the volume of the filtrate, and then the concentrated solution is centrifuged to obtain the biologically active ingredient; the washing method includes rinsing with a NaOH solution with a mass concentration of 11% for 5 times, and then immersing and washing with deionized water for 3 times, and the immersion time is 25 seconds; the amount ratio of mint leaf powder, aloe vera powder and ethanol is 21g:12.5g:200mL;
[0084] (2) Preparation of titanium dioxide: Tetrabutyl titanate was added to ethanol, followed by addition of a 5% Na2CO3 solution, which was condensed and refluxed at 84°C for 9 hours, followed by centrifugation, washing and drying. The amount ratio of ethanol, tetrabutyl titanate and Na2CO3 solution was 70 mL: 0.03 g: 1.5 mL.
[0085] (3) Preparation of biofunctional agent: The bioactive component is dispersed in water, and titanium dioxide, anhydrous ethanol, isopropyl triisostearoyl titanate and polyvinyl pyrrolidone are added thereto and stirred at 70°C to obtain a mixed solution containing the bioactive component. The solution is stirred for 90 minutes and then centrifuged and dried. The weight ratio of the bioactive component, water, titanium dioxide, anhydrous ethanol, isopropyl triisostearoyl titanate and polyvinyl pyrrolidone is 21:70:4:35:7:6.
[0086] Test example: A biofunctional agent was prepared using the aforementioned Examples 1-4 and Comparative Examples 1-8. The biofunctional agent in different examples and PET chips were mixed and melt granulated in a ratio of 1:100 by weight. The mixture was then mixed with commercially available polyester chips and melt-spun to prepare functional polyester fibers, which were then tested as follows.
[0087] 1. Mechanical properties test: The mechanical properties of multifunctional polyester fiber were tested using a multifilament strength and extensometer. The tensile rate of the multifilament strength and extensometer was set to 400 mm / min. -1 , the clamping length is 200mm, the pre-tension is 5cN, and each group of samples is measured 5 times to take the average value;
[0088] 2. Water absorption: Cut the polyester fabric into small square pieces, record its initial mass (M1), put it into a beaker filled with water, and soak it in it for 1 hour. After taking it out, use filter paper to absorb the water on the surface of the fabric until no water drops naturally drip, weigh its mass (M2), and calculate the water absorption rate. Take the average of 3 results and calculate the water absorption rate using the following formula: M = (M2-M1) / M1, where M is the water absorption rate, M1 is the dry weight of the fabric, and M2 is the weight of the fabric after water absorption;
[0089] 3. Air permeability: Tested in accordance with the provisions of GB / T5453-1997;
[0090] 4. Antibacterial performance test: According to the method in GB / T20944.3-2008, the inhibition rate of each group of polyester fibers against Staphylococcus aureus, Escherichia coli, Klebsiella pneumoniae and Candida albicans was tested.
[0091] 5. Washability test: The experiment adopts a bath ratio of 1:30 and a water temperature of 50°C for rinsing for 5 minutes, which is counted as one wash. The antibacterial performance is tested after washing 50 times.
[0092] The test results are shown in Tables 1 and 2 below:
[0093] Table 1
[0094]
[0095] Table 2
[0096]
[0097]
[0098] Finally, it should be noted that the above embodiments are only used to illustrate the present invention and are not intended to limit the technical solutions described in the present invention. Those skilled in the art should understand that the present invention can still be modified or replaced by equivalents. All technical solutions and improvements that do not depart from the spirit and scope of the present invention should be included in the scope of the claims of the present invention.
Claims
1. A method for preparing a biofunctional agent containing a bioactive ingredient, characterized in that the steps include: The bioactive ingredients are dispersed in water, and zeolite-loaded titanium dioxide composite material, anhydrous ethanol, isopropyl triisostearyl titanate and polyvinyl pyrrolidone are added thereto and stirred at a temperature of 65-75° C. to obtain a mixed solution containing the bioactive ingredients, which is stirred for 80-100 minutes and then centrifuged and dried.
2. The method for preparing a biofunctional agent containing a bioactive ingredient according to claim 1, characterized in that: The weight ratio of the bioactive component, water, zeolite-loaded titanium dioxide composite material, anhydrous ethanol, triisostearyl titanate isopropyl and polyvinyl pyrrolidone is (20-22): (60-80): (3-5): (30-40): (6-8): (5-7).
3. The method for preparing a biofunctional agent containing a bioactive ingredient according to claim 1, characterized in that: The preparation method of the bioactive ingredient comprises: washing and drying mint leaves and aloe vera with a water content of less than 5% and crushing them through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder respectively, then mixing them evenly to obtain a mixed powder, adding the mixed powder into ethanol and performing ultrasound for 40-60 minutes, filtering, rotary evaporating and concentrating the filtrate to 30-34% of the volume of the filtrate, and then centrifuging the concentrated solution to obtain the bioactive ingredient.
4. The method for preparing a biofunctional agent containing a bioactive ingredient according to claim 3, characterized in that: The cleaning method comprises washing with a NaOH solution having a mass concentration of 10-12% for 4-6 times, and then immersing and washing with deionized water for 2-4 times, with the immersion time being 20-30 seconds.
5. The method for preparing a biofunctional agent containing a bioactive ingredient according to claim 4, characterized in that: The dosage ratio of the mint leaf powder, aloe powder and ethanol is (20-22) g: (12-13) g: (190-210) mL.
6. The method for preparing a biofunctional agent containing a bioactive ingredient according to claim 1, characterized in that: The preparation method of the zeolite-loaded titanium dioxide composite material comprises: adding zeolite into ethanol and ultrasonically dispersing for 30-40 minutes, adding tetrabutyl titanate at a rotation speed of 200-300 r / min, then adding a Na2CO3 solution with a mass concentration of 4-6% for condensation and reflux, centrifuging, washing and drying to obtain the composite material.
7. The method for preparing a biofunctional agent containing a bioactive component according to claim 6, characterized in that: The dosage ratio of the zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution is (60-80) mg: (60-80) mL: (0.02-0.04) g: (1.4-1.6) mL.
8. The method for preparing a biofunctional agent containing a bioactive component according to claim 6, characterized in that: The condensation reflux temperature is 82-86° C. and the time is 8-10 h.
9. Use of the biofunctional agent prepared by the method for preparing a biofunctional agent containing a bioactive ingredient according to any one of claims 1 to 8 in antibacterial products.
10. The use according to claim 9, characterized in that The antimicrobial product comprises a textile, a fiber or a coating.
Citation Information
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