CN113618078A - Simple method for preparing nano-silver based on frangipani extract - Google Patents
Simple method for preparing nano-silver based on frangipani extract Download PDFInfo
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Abstract
The invention discloses a simple method for preparing nano-silver based on an egg flower extracting solution. Mixing the frangipani ethanol extract with the silver ion solution, and reacting to generate the nano silver. The invention utilizes the frangipani extract to reduce silver ions and prepare simple substance nano silver. According to the method, the nano silver particles with the particle size of 1-57 nm can be prepared. The preparation method is simple and easy to implement, strong in operability and low in cost, the frangipani extract is used as a reducing agent and a stabilizing agent at the same time, other chemical components are not required to be added in the reaction process, a large number of nano silver particles are prepared in a short time, and the preparation method is simple and environment-friendly.
Description
The technical field is as follows:
the invention belongs to the technical field of biology, and particularly relates to a simple method for preparing nano-silver based on an egg flower extracting solution.
Background art:
nano Silver (Silver nanoparticles, Ag-NPs for short) is called as a new generation antibacterial agent in twenty-first century, and has the advantages of broad-spectrum and efficient antibacterial performance, lasting antibacterial property, strong permeability, safety, no toxicity, repair and regeneration, and difficulty in causing microorganisms to generate drug resistance. Nano silver is widely used in various medical materials, such as wound dressing, masks of surgeons, medical catheters, medical surgical instruments, and implanted human tissues. Based on the excellent antibacterial property of the nano-silver, the nano-silver antibacterial material has wide application prospect and has wide market demands in the fields of articles for daily use, medical treatment and health, building materials, electronic industry and the like.
The chemical method for preparing the nano silver comprises the following steps: chemical methods such as a liquid-phase chemical reduction method, an adsorption in-situ reduction method, an ethylene glycol hydrothermal reduction method, an electrochemical method, a photochemical reduction method and the like; the physical method for preparing the nano silver comprises the following steps: reduction ball milling, ultrasonic reduction, microwave-assisted reduction, photon reduction, evaporative condensation, and atomization. The chemical method is common, but the reducing agent and the stabilizing agent are toxic reagents, which seriously pollute the environment, and the reaction conditions need to be strictly controlled, so the preparation technology has very high requirements.
Plumeria rubra (L.cv.acutifolia) genus Apocynaceae family, is distributed in tropical and subtropical regions. The flower is common greening tree species and medicinal plants in the south of China and blooms in summer and autumn. The pharmacological and toxicological research of the frangipani shows that: the plumeria rubra has the pharmacological effects of diminishing inflammation, resisting tumors, promoting wound healing, inhibiting bacteria, inhibiting HIV virus, resisting oxidation, reducing blood fat, relieving fever and pain and the like.
The invention content is as follows:
the invention aims to provide a simple method for preparing nano-silver based on the frangipani extract, which is simple, convenient and easy to implement, strong in operability, low in cost and environment-friendly.
The simple method for preparing the nano-silver based on the frangipani extract comprises the following steps:
mixing the frangipani ethanol extract with the silver ion solution, and reacting to generate the nano silver.
Preferably, the frangipani ethanol extract is the frangipani ethanol extract obtained by drying and crushing frangipani leaves, reflux-extracting the frangipani powder with ethanol water solution, performing ultrasonic treatment and filtering.
Preferably, the method comprises the following specific steps:
(1) washing the frangipani leaf part with water, drying, and crushing by a crusher to obtain frangipani powder;
(2) according to the mass-volume ratio of 1 g: adding 30ml of frangipani powder into ethanol water solution with volume fraction of 70%, carrying out hot reflux at 75 ℃ for 2h, continuously stirring, cooling to room temperature, carrying out ultrasonic treatment under ice bath condition, and filtering to obtain an frangipani ethanol extract;
(3) adding 8-10 mmol/L AgNO3The solution and the frangipani ethanol extract are mixed according to the volume ratio of 2-10: 1, heating and stirring at 60-75 ℃ for reaction for 15 min-1 h to prepare the nano-silver solution.
Preferably, the washing with water of the plumeria rubra leaf part is that the plumeria rubra leaf part is washed with ultrapure water for 3 times.
Preferably, the drying is carried out at 65 ℃ for 1-2 d.
Preferably, the frangipani powder is obtained by crushing the frangipani powder by a crusher and sieving the crushed frangipani powder by a 40-mesh sieve.
Preferably, the ultrasonic treatment under the ice bath condition is carried out under the ice bath condition, the ultrasonic power is 350W, and the ultrasonic treatment is carried out for 20min after 3 sec.
Preferably, the filtered frangipani ethanol extract is filtered by a 0.22 mu M filter membrane.
Preferably, the heating and stirring reaction of step (3) is a reaction protected from light.
The invention utilizes the frangipani extract to reduce silver ions and prepare simple substance nano silver. According to the method, the nano silver particles with the particle size of 1-57 nm can be prepared. The preparation method is simple and easy to implement, strong in operability and low in cost, the frangipani extract is used as a reducing agent and a stabilizing agent at the same time, other chemical components are not required to be added in the reaction process, a large number of nano silver particles are prepared in a short time, and the preparation method is simple and environment-friendly.
The nano-silver synthesized by the frangipani extract has high safety and strong operability. The method for synthesizing the nano-silver by reducing the plant extract has the advantages of local material availability, mild reaction conditions, low cost, low toxicity, difficult agglomeration of products, less pollution and the like. At present, the research on the reduction synthesis of nano-silver by using the frangipani extract is little in China, and the invention is a method for preparing a large amount of nano-silver particles in a short time by using the frangipani extract as a reducing agent and a stabilizing agent at the same time without adding other chemical components.
Drawings
FIG. 1 is an electron micrograph (A) of the nanosilver solution and a particle size distribution (B) of the nanosilver particles of example 1;
FIG. 2 is an electron micrograph (A) of the nanosilver solution and a distribution map (B) of the particle diameters of the nanosilver particles of example 2;
FIG. 3 is the electron micrograph (A) and the particle size distribution (B) of the nano-silver particles of example 3;
FIG. 4 is the electron micrograph (A) and the particle size distribution (B) of the nanosilver solution of example 4;
FIG. 5 is the electron micrograph (A) and the particle size distribution (B) of the nano-silver particles of example 5.
Detailed Description
The following examples are further illustrative of the present invention and are not intended to be limiting thereof.
Example 1:
picking the plumeria rubra leaf part, cleaning with ultrapure water for 3 times, drying at 65 ℃ for 2d, crushing by a crusher, and sieving by a 40-mesh sieve to obtain plumeria rubra powder. Weighing 6g of frangipani powder, adding 180mL of 70% ethanol aqueous solution with volume fraction at 75 ℃, performing hot reflux for 2h, stirring continuously during the hot reflux, and cooling to room temperature; performing ice bath ultrasonic treatment for 20min under ultrasonic condition of 350W for 3sec and 3sec, coarse filtering with 200 mesh gauze, and filtering with 0.22 μ M filter membrane. AgNO with the concentration of 8mmol/L3The volume ratio of the solution to the frangipani extract is 2: 1, heating and stirring at 60 ℃ in a dark place for reaction for 30min to prepare the nano-silver solution.
According to the measurement, as shown in fig. 1, the nano silver solution prepared in this example has a silver ion particle size of 1-36 nm and an average particle size of 10 nm.
Example 2:
picking the plumeria rubra leaf part, cleaning with ultrapure water for 3 times, drying at 65 ℃ for 2d, crushing by a crusher, and sieving by a 40-mesh sieve to obtain plumeria rubra powder. Weighing 6g of frangipani powder, adding 180mL of 70% ethanol aqueous solution with volume fraction, carrying out hot reflux at 75 ℃ for 2h, stirring continuously during the hot reflux, and cooling to room temperature; performing ice bath ultrasonic treatment for 20min under ultrasonic condition of 350W for 3sec and 3sec, coarse filtering with 200 mesh gauze, and filtering with 0.22 μ M filter membrane. AgNO with the concentration of 8mmol/L3The volume ratio of the solution to the frangipani extract is 7: 1, heating and stirring at 70 ℃ in a dark place for reaction for 15min to prepare the nano-silver solution.
According to the measurement, as shown in fig. 2, the nano silver solution prepared in this example has a silver ion particle size of 1-57 nm and an average particle size of 15 nm.
Example 3:
picking the plumeria rubra leaf part, cleaning with ultrapure water for 3 times, drying at 65 ℃ for 2d, crushing by a crusher, and sieving by a 40-mesh sieve to obtain plumeria rubra powder. Weighing 6g of frangipani powder, adding 180mL of 70% ethanol aqueous solution with volume fraction at 75 ℃, performing hot reflux for 2h, stirring continuously during the hot reflux, and cooling to room temperature; performing ice bath ultrasonic treatment for 20min under ultrasonic condition of 350W for 3sec and 3sec, coarse filtering with 200 mesh gauze, and filtering with 0.22 μ M filter membrane. AgNO with the concentration of 8mmol/L3The volume ratio of the solution to the frangipani extract is 8: 1, heating and stirring at 75 ℃ in a dark place for reaction for 1 hour to prepare the nano silver solution.
According to the measurement, as shown in fig. 3, the nano silver solution prepared in this example has a silver ion particle size of 1 to 19nm and an average particle size of 5 nm.
Example 4:
picking the plumeria rubra leaf part, cleaning with ultrapure water for 3 times, drying at 65 ℃ for 2d, crushing by a crusher, and sieving by a 40-mesh sieve to obtain plumeria rubra powder. Weighing 6g of frangipani powder, adding 180mL of 70% ethanol aqueous solution with volume fraction at 75 ℃, performing hot reflux for 2h, stirring continuously during the hot reflux, and cooling to room temperature; performing ice bath ultrasonic treatment for 20min under ultrasonic condition of 350W for 3sec and 3sec, coarse filtering with 200 mesh gauze, and filtering with 0.22 μ M filter membrane. AgNO with the concentration of 10mmol/L3The volume ratio of the solution to the frangipani extract is 9: 1, heating and stirring at 75 ℃ in a dark place for reaction for 1 hour to prepare the nano silver solution.
According to the measurement, as shown in fig. 4, the nano silver solution prepared in this example has a silver ion particle size of 2-22 nm and an average particle size of 8 nm.
Example 5:
picking the plumeria rubra leaf part, cleaning with ultrapure water for 3 times, drying at 65 ℃ for 2d, crushing by a crusher, and sieving by a 40-mesh sieve to obtain plumeria rubra powder. Weighing 6g of frangipani powder, adding 180mL of 70% ethanol aqueous solution with volume fraction at 75 ℃, performing hot reflux for 2h, stirring continuously during the hot reflux, and cooling to room temperature; performing ice bath ultrasonic treatment for 20min under ultrasonic condition of 350W for 3sec and 3sec, coarse filtering with 200 mesh gauze, and filtering with 0.22 μ M filter membrane. AgNO with the concentration of 10mmol/L3The volume ratio of the solution to the frangipani extract is 10: 1, heating and stirring at 75 ℃ in a dark place for reaction for 1 hour to prepare the nano silver solution.
According to the measurement, as shown in fig. 5, the nano silver solution prepared in this example has a silver ion particle size of 1 to 26nm and an average particle size of 7 nm.
The above description is only a preferred embodiment of the present invention, and should not be taken as limiting the scope of the present invention, and the present invention is not limited thereto, and obviously simple modifications, equivalent substitutions, improvements, etc. within the technical spirit of the present invention should be included in the scope of the present invention.
Claims (10)
1. A simple method for preparing nano-silver based on frangipani extract is characterized by comprising the following steps:
mixing the frangipani ethanol extract with the silver ion solution, and reacting to generate the nano silver.
2. The simple method as claimed in claim 1, wherein the said flos Plumeriae Acutifoliae ethanol extract is prepared by drying and pulverizing flos Plumeriae Acutifoliae leaf part, reflux-extracting flos Plumeriae Acutifoliae powder with ethanol water solution, subjecting to ultrasound, and filtering.
3. The simple process of claim 1, wherein the silver ion solution is AgNO3And (3) solution.
4. The simple method according to claim 1, characterized by the specific steps of:
(1) washing the frangipani leaf part with water, drying, and crushing by a crusher to obtain frangipani powder;
(2) according to the mass-volume ratio of 1 g: adding 30ml of frangipani powder into ethanol water solution with volume fraction of 70%, carrying out hot reflux at 75 ℃ for 2h, continuously stirring, cooling to room temperature, carrying out ultrasonic treatment under ice bath condition, and filtering to obtain an frangipani ethanol extract;
(3) adding 8-10 mmol/L AgNO3The solution and the frangipani ethanol extract are mixed according to the volume ratio of 2-10: 1, heating and stirring at 60-75 ℃ for reaction for 15 min-1 h to prepare the nano-silver solution.
5. The simple method as claimed in claim 4, wherein the washing with water of the plumeria rubra leaf part is carried out 3 times by washing the plumeria rubra leaf part with ultra pure water.
6. The simple method of claim 4, wherein the drying is drying at 65 ℃ for 1-2 days.
7. The simple method as claimed in claim 4, wherein the frangipani powder is obtained by pulverizing with a pulverizer and sieving with a 40 mesh sieve.
8. The simple method as claimed in claim 4, wherein the ultrasound under ice bath condition is ultrasound under ice bath condition with ultrasonic power of 350W and ultrasonic power of 3sec for 20 min.
9. The simple method as claimed in claim 4, wherein the ethanol extract of frangipani is filtered through a 0.22 μ M membrane.
10. The simple method as claimed in claim 4, wherein the heating and stirring reaction of step (3) is a reaction protected from light.
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Cited By (2)
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| CN114734032A (en) * | 2022-04-27 | 2022-07-12 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Method for preparing nano-silver based on kapok extract |
| WO2023070967A1 (en) * | 2021-10-28 | 2023-05-04 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Method for preparing silver nanoparticles on basis of amaranthus tricolor l extract |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2023070967A1 (en) * | 2021-10-28 | 2023-05-04 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Method for preparing silver nanoparticles on basis of amaranthus tricolor l extract |
| CN114734032A (en) * | 2022-04-27 | 2022-07-12 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Method for preparing nano-silver based on kapok extract |
| CN114734032B (en) * | 2022-04-27 | 2024-02-20 | 广东省科学院微生物研究所(广东省微生物分析检测中心) | Method for preparing nano silver based on kapok extract |
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