Preparation method and application of a biological functional agent containing a bioactive ingredient

Abstract

The present invention provides a preparation method of a biological functional agent containing a bioactive ingredient. The steps include: dispersing the bioactive ingredient in water, and adding a zeolite-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate, and polyvinylpyrrolidone thereto, and stirring at a temperature of 65-75 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 80-100 min, centrifuging and drying are carried out to obtain the product. The preparation method of the biological functional agent containing the bioactive ingredient provided by the present invention improves the loading amount of the bioactive ingredient on the carrier, enhances the stability of the bioactive ingredient, and strengthens the sustained-release effect. This not only improves the preparation efficiency and performance of the biological functional agent, but also provides broad prospects for its application in the fields of medicine, cosmetics, environmental protection, etc.

Description

Technical Field

[0001] The present invention relates to the technical field of biological functional agents, and particularly relates to a preparation method of a biological functional agent containing biological active ingredients. Background Art

[0002] Under the background of the development of modern science and technology, the preparation and application of biological functional agents have gradually become research hotspots. Due to the presence of specific biological active ingredients, such functional agents are widely used in multiple fields such as medicine, environmental protection, and materials science. Biological functional agents are usually prepared by extracting and purifying biological active ingredients existing in nature. These biological active ingredients have various functions such as antiviral, antibacterial, and antioxidant. Therefore, it is of great significance to develop functional agents containing these ingredients.

[0003] In the preparation process, it is first necessary to extract the required biological active ingredients 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 biological active ingredients. Purification is to remove impurities in the extract and improve the purity and stability of the biological active ingredients. Commonly used purification methods include crystallization, chromatography, membrane separation, etc. Through purification, biological active ingredients with higher purity can be obtained, laying a good foundation for the subsequent preparation of functional agents.

[0004] When preparing biological functional agents, it is usually necessary to compound the purified biological active ingredients with other substances to improve their stability and application scope. For example, the biological active ingredients can be compounded with polymers, inorganic materials, etc. to form functional agents with specific properties. In addition, technologies such as molecular capsules and molecular nests can be used to encapsulate and protect the biological active 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 biological functional agents. For example, using nanotechnology, biological active ingredients can be prepared into nanoparticles to improve their solubility and biological activity; using biotechnology, microbial communities with specific functions can be constructed for the preparation of biological functional agents with special properties.

[0006] In terms of specific applications, biological functional agents containing biological active ingredients have broad application prospects in the medical field. For example, drugs with antiviral and antibacterial functions can be prepared; in the environmental protection field, biological functional agents for degrading organic pollutants can be prepared; in the materials science field, biological composite materials with special properties can be prepared. Based on this, the present invention provides a preparation method of a biological functional agent containing biological active ingredients. Summary of the Invention

[0007] The object of the present invention is to provide a preparation method of a bio-functional agent containing a bioactive ingredient, which improves the loading amount of the bioactive ingredient on the carrier, enhances the stability of the bioactive ingredient, and strengthens the sustained-release effect.

[0008] On the one hand, the present invention provides a preparation method of a bio-functional agent containing a bioactive ingredient. The steps include: dispersing the bioactive ingredient in water, and adding a zeolite-supported titanium dioxide composite material, absolute ethanol, triisostearoyl titanate isopropyl ester, and polyvinylpyrrolidone thereto, and stirring at a temperature of 65-75 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 80-100 min, centrifuging and drying are carried out to obtain the product.

[0009] Further, the weight ratio of the bioactive ingredient, water, zeolite-supported titanium dioxide composite material, absolute ethanol, triisostearoyl titanate isopropyl ester, and polyvinylpyrrolidone is (20-22):

[0010] (60-80):(3-5):(30-40):(6-8):(5-7).

[0011] Further, the preparation method of the bioactive ingredient includes: respectively pulverizing mint leaves and aloe vera that have been cleaned and dried to a water content of less than 5% 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 to ethanol for ultrasonic treatment for 40-60 min, filtering, and then rotary evaporating and concentrating the filtrate to 30-34% of the original volume of the filtrate, and then centrifuging the concentrated solution to obtain the product.

[0012] Further, the cleaning method includes rinsing with a NaOH solution with a mass concentration of 10-12% for 4-6 times, and then impregnating and washing with deionized water for 2-4 times, and the impregnation time is 20-30 s.

[0013] Further, the dosage ratio of the mint leaf powder, aloe vera powder, and ethanol is (20-22) g:(12-13) g:(190-210) mL.

[0014] Further, the preparation method of the zeolite-supported titanium dioxide composite material includes: adding zeolite to ethanol and ultrasonically dispersing it for 30-40 min, adding tetrabutyl titanate under the condition of a rotation speed of 200-300 r / min, then adding a Na2CO3 solution with a mass concentration of 4-6% for condensation reflux, centrifuging, washing, and drying to obtain the product.

[0015] Further, 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.

[0016] Further, the temperature of the condensation reflux is 82 - 86 °C, and the time is 8 - 10 h.

[0017] On the other hand, the present invention also provides the application of a bio - functional agent prepared by a preparation method of a bio - functional agent containing bioactive components in an antibacterial product.

[0018] Further, the antibacterial product includes textiles, fibers or coatings.

[0019] The beneficial effects of the present invention are as follows:

[0020] (1) In the present invention, the bioactive components include the compound of peppermint leaves and aloe powder. Both of these two plants contain rich bioactive components, such as menthol, aloe polysaccharide, etc., which have extensive medical and health care values. When the two are compounded, hydrogen bonds are formed between the alcohol, ketone and other components in the peppermint leaves and the polysaccharide, organic acid and other components in the aloe powder, which can stabilize the structure of the compound, prevent the mutual collision and decomposition between molecules. At the same time, they may also protect each other through steric hindrance effects, making the entire compounding system more stable, which is beneficial to the preservation and release of bioactive components;

[0021] (2) The extraction method of the bioactive components of aloe powder in the present invention is simple, and it directly uses the methods of drying and pulverizing. It has certain water absorption, and can improve the air permeability of the material when combined with mint active components. This is mainly due to the porous structure of aloe powder and the volatility of mint components. The porous structure of aloe powder makes it have good air permeability, allowing the free passage of air and water molecules; in addition, the aloe active components can also have a certain high - temperature resistance to a certain extent, which is mainly related to its chemical structure and stability; the bioactive 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) The bio - functional agent prepared in the present invention has a high inhibition rate against Staphylococcus aureus, Escherichia coli, Klebsiella pneumoniae and Candida albicans after being prepared into polyester fibers; the components such as menthol and menthone in peppermint leaves and the polysaccharides and anthraquinone compounds in aloe all have significant antibacterial activities. These components can destroy the cell wall or cell membrane of bacteria and inhibit their growth and reproduction; the interaction after the two are mixed can enhance each other's antibacterial effect;

[0023] (4) The present invention uses a zeolite-supported titanium dioxide composite material as a carrier to load bioactive components, which has slow-release controllability. Furthermore, during high-temperature water washing, the active sites can still adsorb and fix the aloe active components, making them not easily washed away by the water flow. In addition, when the mint powder and aloe powder are compounded, the active components in the mint powder interact with the active sites on the surface of the zeolite-supported 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 components, enhancing the binding force between the two. Therefore, the functional polyester fiber prepared with the bio-functional agent can still maintain a good bactericidal effect after being washed at 50°C.

[0024] (5) When the zeolite-supported titanium dioxide composite material is used as a carrier, the porous structure of the zeolite is utilized. These micropores and mesopores are like tiny "storerooms", providing abundant adsorption sites for bioactive components. By introducing titanium dioxide, not only the surface properties of the zeolite are optimized, but also the interaction force between the zeolite and bioactive components is enhanced, thereby greatly increasing the loading amount of bioactive components on the composite material. This means that each unit mass of the composite material can carry more bioactive components, improving the overall efficiency of the material. The combination of the porous structure of the zeolite and the coating effect of titanium dioxide provides a fine regulation mechanism for the release of bioactive components, realizing a slow and continuous release of bioactive components. This slow-release characteristic not only prolongs the action time of bioactive components but also improves the utilization rate of bioactive components.

[0025] (6) The bio-functional agent prepared in the present invention has excellent slow-release performance and bactericidal performance, and its application can be extended to products such as textiles, masks, and coatings. Specific Embodiments

[0026] The technical solutions of the present invention will be described clearly and completely below. Obviously, the described embodiments are some, but not all, of the embodiments of the present invention. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention. The raw materials not described in the following embodiments are all commercially available.

[0027] Example 1

[0028] This example provides a preparation method of a bio-functional agent containing bioactive components. The steps include:

[0029] (1) Preparation of bioactive components: Wash and dry peppermint leaves and aloe vera until the water content is less than 5%, then crush them through a 60-mesh sieve to obtain peppermint leaf powder and aloe vera powder. Subsequently, mix them evenly to obtain a mixed powder. Take the mixed powder and add it to ethanol for ultrasonic treatment for 50 min. After filtration, rotate and evaporate the filtrate to concentrate it to 32% of the original volume of the filtrate. Then, centrifuge the concentrated solution to obtain the product; the washing method includes rinsing 5 times with a NaOH solution with a mass concentration of 11%, and then impregnating and washing 3 times with deionized water, with an impregnation time of 25 s; the dosage ratio of peppermint leaf powder, aloe vera powder and ethanol is 21 g: 12.5 g: 200 mL;

[0030] (2) Preparation of zeolite-supported titanium dioxide composite: Add zeolite to ethanol and disperse it by ultrasonic treatment for 35 min. Add tetrabutyl titanate under the condition of a rotation speed of 250 r / min. Subsequently, add a Na2CO3 solution with a mass concentration of 5% and carry out condensation reflux at a temperature of 84 °C for 9 h. After centrifugation and washing, dry it to obtain the product; the dosage ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution is 70 mg: 70 mL: 0.03 g: 1.5 mL;

[0031] (3) Preparation of bio-functional agent: Disperse the bioactive components in water, and add zeolite-supported titanium dioxide composite, anhydrous ethanol, triisostearoyl titanate and polyvinylpyrrolidone to it, and stir at a temperature of 70 °C to obtain a mixed solution containing bioactive components. After stirring for 90 min, centrifuge and dry it to obtain the product; the weight ratio of bioactive components, water, zeolite-supported titanium dioxide composite, anhydrous ethanol, triisostearoyl titanate and polyvinylpyrrolidone is 21: 70: 4: 35: 7: 6.

[0032] Example 2

[0033] This example provides a preparation method of a bio-functional agent containing bioactive components, and the steps include:

[0034] (1) Preparation of bioactive components: Wash and dry peppermint leaves and aloe vera until the water content is less than 5%, then crush them through a 60-mesh sieve to obtain peppermint leaf powder and aloe vera powder. Subsequently, mix them evenly to obtain a mixed powder. Take the mixed powder and add it to ethanol for ultrasonic treatment for 40 min. After filtration, rotate and evaporate the filtrate to concentrate it to 30% of the original volume of the filtrate. Then, centrifuge the concentrated solution to obtain the product; the washing method includes rinsing 4 times with a NaOH solution with a mass concentration of 10%, and then impregnating and washing 2 times with deionized water, with an impregnation time of 20 s; the dosage ratio of peppermint leaf powder, aloe vera powder and ethanol is 20 g: 12 g: 190 mL;

[0035] (2) Preparation of zeolite-supported titanium dioxide composite: Add zeolite into ethanol and ultrasonically disperse it for 30 min. Add tetrabutyl titanate under the condition of a rotation speed of 200 r / min. Subsequently, add a Na2CO3 solution with a mass concentration of 4% and carry out reflux condensation at 82 °C for 8 h. After centrifugation and washing, dry it to obtain; the dosage ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution is 60 mg: 60 mL: 0.02 g: 1.4 mL;

[0036] (3) Preparation of bio-functional agent: Disperse the bioactive ingredient in water, and add zeolite-supported titanium dioxide composite, absolute ethanol, isostearoyl titanate isopropyl ester and polyvinylpyrrolidone thereto, and stir at 65 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 80 min, centrifuge and dry it to obtain; the weight part ratio of the bioactive ingredient, water, zeolite-supported titanium dioxide composite, absolute ethanol, isostearoyl titanate isopropyl ester and polyvinylpyrrolidone is 20: 60: 3: 30: 6: 5.

[0037] Example 3

[0038] This example provides a preparation method of a bio-functional agent containing a bioactive ingredient, and the steps include:

[0039] (1) Preparation of bioactive ingredient: Crush the mint leaves and aloe vera that have been cleaned and dried to a water content of less than 5% through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder. Subsequently, mix them evenly to obtain a mixed powder. Take the mixed powder and add it to ethanol for ultrasonic treatment for 60 min. After filtration, rotate and evaporate the filtrate to concentrate it to 34% of the original volume of the filtrate. Subsequently, centrifuge the concentrated solution to obtain; the cleaning method includes rinsing 6 times with a NaOH solution with a mass concentration of 12%, and then impregnating and washing 4 times with deionized water, and the impregnation time is 30 s; the dosage ratio of mint leaf powder, aloe vera powder and ethanol is 22 g: 13 g: 210 mL;

[0040] (2) Preparation of zeolite-supported titanium dioxide composite: Add zeolite into ethanol and ultrasonically disperse it for 40 min. Add tetrabutyl titanate under the condition of a rotation speed of 300 r / min. Subsequently, add a Na2CO3 solution with a mass concentration of 6% and carry out reflux condensation at 86 °C for 10 h. After centrifugation and washing, dry it to obtain; the dosage ratio of zeolite, ethanol, tetrabutyl titanate and Na2CO3 solution is 80 mg: 80 mL: 0.04 g: 1.6 mL;

[0041] (3) Preparation of the biological functional agent: Disperse the bioactive ingredient in water, and add the zeolite-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate, and polyvinylpyrrolidone thereto, and stir at a temperature of 75 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 100 min, centrifuge and dry to obtain it; the weight ratio of the bioactive ingredient, water, zeolite-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate, and polyvinylpyrrolidone is 22:80:5:40:8:7.

[0042] Example 4

[0043] This example provides a preparation method of a biological functional agent containing a bioactive ingredient, and the steps include:

[0044] (1) Preparation of the bioactive ingredient: Crush the mint leaves and aloe vera that have been washed and dried to a water content of less than 5% through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, and then mix them evenly to obtain a mixed powder. Take the mixed powder and add it to ethanol for ultrasonic treatment for 40 min. After filtration, rotate and evaporate the filtrate to concentrate it to 34% of the original volume of the filtrate, and then centrifuge the concentrated solution to obtain it; the cleaning method includes rinsing 6 times with a 10% NaOH solution by mass concentration, and then impregnating and washing 2 times with deionized water, and the impregnation time is 30 s; the dosage ratio of the mint leaf powder, aloe vera powder, and ethanol is 20 g:13 g:190 mL;

[0045] (2) Preparation of the zeolite-supported titanium dioxide composite material: Add zeolite to ethanol and disperse it by ultrasonic treatment for 40 min. Add tetrabutyl titanate under the condition of a rotation speed of 200 r / min, and then add a 6% Na2CO3 solution by mass concentration and carry out condensation reflux at a temperature of 82 °C for 10 h. After centrifugation, washing, and drying, obtain it; the dosage ratio of zeolite, ethanol, tetrabutyl titanate, and Na2CO3 solution is 60 mg:80 mL:0.02 g:1.6 mL;

[0046] (3) Preparation of the biological functional agent: Disperse the bioactive ingredient in water, and add the zeolite-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate, and polyvinylpyrrolidone thereto, and stir at a temperature of 65 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 100 min, centrifuge and dry to obtain it; the weight ratio of the bioactive ingredient, water, zeolite-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate, and polyvinylpyrrolidone is 20:80:3:40:6:7.

[0047] Comparative Example 1

[0048] This comparative example provides a preparation method of a biological functional agent containing a bioactive ingredient, and the steps include:

[0049] (1) Preparation of bioactive ingredient: Aloe vera that has been cleaned and dried to a water content of less than 5% is pulverized and passed through a 60-mesh sieve to obtain aloe vera powder. The powder is added to ethanol and ultrasonicated for 50 min. After filtration, the filtrate is rotary evaporated and concentrated to 32% of the original volume. Subsequently, the concentrated solution is centrifuged to obtain the product; the cleaning method includes rinsing 5 times with a NaOH solution with a mass concentration of 11%, and then impregnating and washing 3 times with deionized water, with an impregnation time of 25 s; the dosage ratio of aloe vera powder to ethanol is 33.5 g: 200 mL;

[0050] (2) Preparation of zeolite-supported titanium dioxide composite: Zeolite is added to ethanol and ultrasonicated for 35 min. Tetrabutyl titanate is added under the condition of a rotation speed of 250 r / min. Subsequently, a Na2CO3 solution with a mass concentration of 5% is added, and the mixture is refluxed under condensation at 84 °C for 9 h. After centrifugation, washing, and drying, the product is obtained; the dosage ratio of zeolite, ethanol, tetrabutyl titanate, and Na2CO3 solution is 70 mg: 70 mL: 0.03 g: 1.5 mL;

[0051] (3) Preparation of bio-functional agent: The bioactive ingredient is dispersed in water, and zeolite-supported titanium dioxide composite, absolute ethanol, triisostearoyl titanate, and polyvinylpyrrolidone are added thereto. The mixture is stirred at 70 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 90 min, it is centrifuged and dried to obtain the product; the weight ratio of the bioactive ingredient, water, zeolite-supported titanium dioxide composite, absolute ethanol, triisostearoyl titanate, and polyvinylpyrrolidone is 21: 70: 4: 35: 7: 6.

[0052] Comparative Example 2

[0053] This comparative example provides a preparation method of a bio-functional agent containing a bioactive ingredient. The steps include:

[0054] (1) Preparation of bioactive ingredient: Peppermint leaves that have been cleaned and dried to a water content of less than 5% are pulverized and passed through a 60-mesh sieve to obtain peppermint leaf powder. Subsequently, it is added to ethanol and ultrasonicated for 50 min. After filtration, the filtrate is rotary evaporated and concentrated to 32% of the original volume. Subsequently, the concentrated solution is centrifuged to obtain peppermint leaf extract, which is then mixed with aloe vera extract powder purchased from Weiyi Peptide (Guangdong) Biotechnology Co., Ltd. to obtain the product, wherein the ratio of peppermint leaf extract to aloe vera extract is 21: 12.5; the cleaning method includes rinsing 5 times with a NaOH solution with a mass concentration of 11%, and then impregnating and washing 3 times with deionized water, with an impregnation time of 25 s; the dosage ratio of peppermint leaf powder to ethanol is 33.5 g: 200 mL;

[0055] (2) Preparation of zeolite-supported titanium dioxide composite: Add zeolite into ethanol and ultrasonically disperse for 35 min. Add tetrabutyl titanate under the condition of a rotation speed of 250 r / min. Subsequently, add a 5% (by mass) Na2CO3 solution and carry out reflux condensation at 84 °C for 9 h. After centrifugation and washing, dry to obtain the product. The dosage ratio of zeolite, ethanol, tetrabutyl titanate, and Na2CO3 solution is 70 mg: 70 mL: 0.03 g: 1.5 mL;

[0056] (3) Preparation of bio-functional agent: Disperse the bioactive ingredient in water, and add zeolite-supported titanium dioxide composite, absolute ethanol, isostearoyl titanate isopropyl ester, and polyvinylpyrrolidone thereto. Stir at 70 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 90 min, centrifuge and dry to obtain the product. The weight ratio of the bioactive ingredient, water, zeolite-supported titanium dioxide composite, absolute ethanol, isostearoyl titanate isopropyl ester, and polyvinylpyrrolidone is 21: 70: 4: 35: 7: 6.

[0057] Comparative Example 3

[0058] This comparative example provides a preparation method of a bio-functional agent containing a bioactive ingredient. The steps include:

[0059] (1) Preparation of bioactive ingredient: Crush mint leaves that have been cleaned and dried to a water content of less than 5% through a 60-mesh sieve to obtain mint leaf powder. Take the powder, add it to ethanol, and ultrasonically treat for 50 min. After filtration, rotary evaporate and concentrate the filtrate to 32% of the original volume of the filtrate. Subsequently, centrifuge the concentrated solution to obtain the product. The cleaning method includes rinsing 5 times with an 11% (by mass) NaOH solution, and then impregnating and washing 3 times with deionized water, with an impregnation time of 25 s. The dosage ratio of mint leaf powder and ethanol is 33.5 g: 200 mL;

[0060] (2) Preparation of zeolite-supported titanium dioxide composite: Add zeolite into ethanol and ultrasonically disperse for 35 min. Add tetrabutyl titanate under the condition of a rotation speed of 250 r / min. Subsequently, add a 5% (by mass) Na2CO3 solution and carry out reflux condensation at 84 °C for 9 h. After centrifugation and washing, dry to obtain the product. The dosage ratio of zeolite, ethanol, tetrabutyl titanate, and Na2CO3 solution is 70 mg: 70 mL: 0.03 g: 1.5 mL;

[0061] (3) Preparation of the biological functional agent: Disperse the bioactive ingredient in water, and add the zeolite-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate, and polyvinylpyrrolidone thereto, and stir at a temperature of 70 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 90 min, centrifuge and dry to obtain it; the weight ratio of the bioactive ingredient, water, zeolite-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate, and polyvinylpyrrolidone is 21:70:4:35:7:6.

[0062] Comparative Example 4

[0063] This comparative example provides a preparation method of a biological functional agent containing a bioactive ingredient, and the steps include:

[0064] (1) Preparation of the bioactive ingredient: Crush wormwood and aloe vera that have been washed and dried to a water content of less than 5% through a 60-mesh sieve to obtain wormwood powder and aloe vera powder, and then mix them evenly to obtain a mixed powder. Take the mixed powder and add it to ethanol for ultrasonic treatment for 50 min. After filtration, rotate and evaporate the filtrate to concentrate it to 32% of the original volume of the filtrate, and then centrifuge the concentrated solution to obtain it; the washing method includes rinsing 5 times with a NaOH solution with a mass concentration of 11%, and then impregnating and washing 3 times with deionized water, and the impregnation time is 25 s; the dosage ratio of wormwood powder, aloe vera powder, and ethanol is 21 g:12.5 g:200 mL;

[0065] (2) Preparation of the zeolite-supported titanium dioxide composite material: Add zeolite to ethanol and disperse it by ultrasonic treatment for 35 min. Add tetrabutyl titanate under the condition of a rotation speed of 250 r / min, and then add a Na2CO3 solution with a mass concentration of 5% and carry out reflux condensation at a temperature of 84 °C for 9 h. After centrifugation, washing, and drying, obtain it; the dosage ratio of zeolite, ethanol, tetrabutyl titanate, and Na2CO3 solution is 70 mg:70 mL:0.03 g:1.5 mL;

[0066] (3) Preparation of the biological functional agent: Disperse the bioactive ingredient in water, and add the zeolite-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate, and polyvinylpyrrolidone thereto, and stir at a temperature of 70 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 90 min, centrifuge and dry to obtain it; the weight ratio of the bioactive ingredient, water, zeolite-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate, and polyvinylpyrrolidone is 21:70:4:35:7:6.

[0067] Comparative Example 5

[0068] This comparative example provides a preparation method of a biological functional agent containing a bioactive ingredient, and the steps include:

[0069] (1) Preparation of bioactive components: The mint leaves and aloe vera that have been cleaned and dried to a water content of less than 5% are respectively crushed through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder. Then, they are mixed evenly to obtain a mixed powder. Take the mixed powder and add it to ethanol for ultrasonic treatment for 50 minutes. After filtration, the filtrate is rotary evaporated and concentrated to 32% of the original volume of the filtrate. Then, the concentrated solution is centrifuged to obtain the bioactive components. The cleaning method includes rinsing 5 times with a NaOH solution with a mass concentration of 11%, and then impregnating and washing 3 times with deionized water, with an impregnation time of 25 seconds. The dosage ratio of mint leaf powder, aloe vera powder, and ethanol is 21 g: 12.5 g: 200 mL.

[0070] (2) Preparation of bio-functional agent: Disperse the bioactive components in water, and add zeolite, absolute ethanol, isopropyl triisostearoyl titanate, and polyvinylpyrrolidone thereto, and stir at a temperature of 70 °C to obtain a mixed solution containing bioactive components. After stirring for 90 minutes, centrifuge and dry to obtain the bio-functional agent. The weight part ratio of bioactive components, water, zeolite, absolute ethanol, isopropyl triisostearoyl titanate, and polyvinylpyrrolidone is 21: 70: 4: 35: 7: 6.

[0071] Comparative Example 6

[0072] This comparative example provides a preparation method of a bio-functional agent containing bioactive components, and the steps include:

[0073] (1) Preparation of bioactive components: The mint leaves and aloe vera that have been cleaned and dried to a water content of less than 5% are respectively crushed through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder. Then, they are mixed evenly to obtain a mixed powder. Take the mixed powder and add it to ethanol for ultrasonic treatment for 50 minutes. After filtration, the filtrate is rotary evaporated and concentrated to 32% of the original volume of the filtrate. Then, the concentrated solution is centrifuged to obtain the bioactive components. The cleaning method includes rinsing 5 times with a NaOH solution with a mass concentration of 11%, and then impregnating and washing 3 times with deionized water, with an impregnation time of 25 seconds. The dosage ratio of mint leaf powder, aloe vera powder, and ethanol is 21 g: 12.5 g: 200 mL.

[0074] (2) Preparation of zeolite-supported silica composite material: Add zeolite to ethanol and ultrasonically disperse it for 35 minutes. Add tetraethyl orthosilicate under the condition of a rotation speed of 250 r / min, and then add ammonia water to adjust the pH to 8 - 12. Stir magnetically at normal temperature and in a closed state for 2 - 7 hours, and then centrifuge, wash, and dry to obtain the zeolite-supported silica composite material. The dosage ratio of zeolite, ethanol, and tetraethyl orthosilicate is 70 mg: 140 mL: 0.03 g.

[0075] (3) Preparation of the biological functional agent: Disperse the bioactive ingredient in water, and add the zeolite-supported silica composite material, anhydrous ethanol, triisostearoyl titanate isopropyl ester, and polyvinylpyrrolidone thereto, and stir at 70 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 90 min, centrifuge and dry to obtain it; the weight ratio of the bioactive ingredient, water, zeolite-supported silica composite material, anhydrous ethanol, triisostearoyl titanate isopropyl ester, and polyvinylpyrrolidone is 21:70:4:35:7:6.

[0076] Comparative Example 7

[0077] This comparative example provides a preparation method of a biological functional agent containing a bioactive ingredient. The steps include:

[0078] (1) Preparation of the bioactive ingredient: Crush the mint leaves and aloe vera that have been cleaned and dried to a water content of less than 5% through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, and then mix them evenly to obtain a mixed powder. Take the mixed powder and add it to ethanol for ultrasonic treatment for 50 min. After filtration, rotate and evaporate the filtrate to concentrate it to 32% of the original volume of the filtrate, and then centrifuge the concentrated solution to obtain it; the cleaning method includes rinsing 5 times with a NaOH solution with a mass concentration of 11%, and then impregnating and washing 3 times with deionized water, and the impregnation time is 25 s; the dosage ratio of the mint leaf powder, aloe vera powder, and ethanol is 21 g:12.5 g:200 mL;

[0079] (2) Preparation of the silica-supported titanium dioxide composite material: Add zeolite to ethanol and disperse it by ultrasonic treatment for 35 min. Add tetrabutyl titanate under the condition of a rotation speed of 250 r / min, and then add a Na2CO3 solution with a mass concentration of 5% and carry out condensation reflux at 84 °C for 9 h. After centrifugation and washing, dry to obtain it; the dosage ratio of zeolite, ethanol, tetrabutyl titanate, and Na2CO3 solution is 70 mg:70 mL:0.03 g:1.5 mL;

[0080] (3) Preparation of the biological functional agent: Disperse the bioactive ingredient in water, and add the silica-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl ester, and polyvinylpyrrolidone thereto, and stir at 70 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 90 min, centrifuge and dry to obtain it; the weight ratio of the bioactive ingredient, water, silica-supported titanium dioxide composite material, anhydrous ethanol, triisostearoyl titanate isopropyl ester, and polyvinylpyrrolidone is 21:70:4:35:7:6.

[0081] Comparative Example 8

[0082] This comparative example provides a preparation method of a biological functional agent containing a bioactive ingredient. The steps include:

[0083] (1) Preparation of bioactive components: The mint leaves and aloe vera that have been cleaned and dried to a water content of less than 5% are respectively pulverized through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder. Subsequently, they are mixed evenly to obtain a mixed powder. The mixed powder is added to ethanol and ultrasonicated for 50 min. After filtration, the filtrate is rotary evaporated and concentrated to 32% of the original volume. Then, the concentrated solution is centrifuged to obtain the bioactive components. The cleaning method includes rinsing 5 times with a NaOH solution with a mass concentration of 11%, and then impregnating and washing 3 times with deionized water, with an impregnation time of 25 s. The dosage ratio of mint leaf powder, aloe vera powder, and ethanol is 21 g: 12.5 g: 200 mL.

[0084] (2) Preparation of titanium dioxide: Tetrabutyl titanate is added to ethanol, and then a Na2CO3 solution with a mass concentration of 5% is added. The mixture is refluxed under condensation at 84 °C for 9 h, and then centrifuged, washed, and dried to obtain titanium dioxide. The dosage ratio of ethanol, tetrabutyl titanate, and Na2CO3 solution is 70 mL: 0.03 g: 1.5 mL.

[0085] (3) Preparation of bio-functional agent: The bioactive components are dispersed in water, and titanium dioxide, absolute ethanol, isopropyl triisostearoyl titanate, and polyvinylpyrrolidone are added thereto. The mixture is stirred at 70 °C to obtain a mixed solution containing bioactive components. After stirring for 90 min, it is centrifuged and dried to obtain the bio-functional agent. The weight ratio of bioactive components, water, titanium dioxide, absolute ethanol, isopropyl triisostearoyl titanate, and polyvinylpyrrolidone is 21: 70: 4: 35: 7: 6.

[0086] Test example: The bio-functional agents prepared by using the foregoing Examples 1-4 and Comparative Examples 1-8 are taken. Bio-functional agents and PET chips in different examples with a weight ratio of 1: 100 are mixed and melt granulated. Then, they are mixed with commercially available polyester chips and melt spun to prepare functional polyester fibers. Subsequently, the following tests are carried out.

[0087] 1. Mechanical property test: A multifilament strength and elongation tester is used to test the mechanical properties of the functional polyester fibers. Set the tensile rate of the multifilament strength and elongation tester to 400 mm·min -1 , the clamping length is 200 mm, the pre-tension is 5 cN, and each group of samples is measured 5 times and the average value is taken;

[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 for 1 h. After taking it out, use filter paper to absorb the water on the surface of the fabric until no water droplets drip naturally, weigh its mass (M2), and calculate the water absorption rate. Take the average value of 3 results. The water absorption rate is calculated by 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: The test is carried out in accordance with the provisions of Standard GB / T5453-1997.

[0090] 4. Antibacterial performance test: According to the method in GB / T20944.3-2008, the inhibition rates of each group of polyester fibers against Staphylococcus aureus, Escherichia coli, Klebsiella pneumoniae and Candida albicans are tested.

[0091] 5. Wash resistance test: In the experiment, the bath ratio is 1:30, the water temperature is 50°C, and it is rinsed for 5 minutes, which is counted as 1 wash. After washing 50 times, the antibacterial performance is tested.

[0092] The test results are shown in Table 1 and Table 2 as follows:

[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 do not limit the technical solutions described in the present invention; those of ordinary skill in the art should understand that the present invention can still be modified or equivalently replaced; and all technical solutions and their improvements that do not depart from the spirit and scope of the present invention should be covered by the scope of the claims of the present invention.

Claims

1. A preparation method of a bio-functional agent containing bioactive components, characterized in that the steps Comprising: Disperse the bioactive ingredient in water, and add zeolite-supported titanium dioxide composite, absolute ethanol, triisostearoyl titanate and polyvinylpyrrolidone thereto, and stir at a temperature of 65-75 °C to obtain a mixed solution containing the bioactive ingredient. After stirring for 80-100 min, centrifuge and dry to obtain; The weight ratio of the bioactive ingredient, water, zeolite-supported titanium dioxide composite, absolute ethanol, triisostearoyl titanate and polyvinylpyrrolidone is (20-22):(60-80):(3-5):(30-40):(6-8):(5-7); The preparation method of the bioactive ingredient includes: crushing the mint leaves and aloe vera that have been washed and dried to a water content of less than 5% through a 60-mesh sieve to obtain mint leaf powder and aloe vera powder, then mixing evenly to obtain a mixed powder, taking the mixed powder and adding it to ethanol for ultrasonic treatment for 40-60 min, filtering, and rotary evaporating and concentrating the filtrate to 30-34% of the original volume of the filtrate, and then centrifuging the concentrated solution to obtain; The cleaning method includes rinsing 4-6 times with a NaOH solution with a mass concentration of 10-12%, and then soaking and washing 2-4 times with deionized water, and the soaking time is 20-30 s; The dosage ratio of the mint leaf powder, aloe vera powder and ethanol is (20-22) g:(12-13) g:(190-210) mL.

2. The preparation method of a bio-functional agent containing a bioactive ingredient according to claim 1, characterized in that, The preparation method of the zeolite-supported titanium dioxide composite includes: adding zeolite to ethanol and ultrasonically dispersing for 30-40 min, adding tetrabutyl titanate under the condition of a rotation speed of 200-300 r / min, and then adding a Na2CO3 solution with a mass concentration of 4-6% for reflux condensation, centrifuging, washing and drying to obtain.

3. The preparation method of a bio-functional agent containing a bioactive ingredient according to claim 2, 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.

4. The preparation method of a bio-functional agent containing a bioactive ingredient according to claim 2, characterized in that, The temperature of the reflux condensation is 82-86 °C, and the time is 8-10 h.

5. Application of the bio-functional agent prepared by the preparation method of the bio-functional agent containing a bioactive ingredient according to any one of claims 1-4 in an antibacterial product.

6. The application according to claim 5, characterized in that The antibacterial product includes textiles, fibers or coatings.

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