CN113084182A - Method for preparing nano-silver by using tea leaching solution as raw material - Google Patents

Method for preparing nano-silver by using tea leaching solution as raw material Download PDF

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Publication number
CN113084182A
CN113084182A CN202110241811.0A CN202110241811A CN113084182A CN 113084182 A CN113084182 A CN 113084182A CN 202110241811 A CN202110241811 A CN 202110241811A CN 113084182 A CN113084182 A CN 113084182A
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CN
China
Prior art keywords
tea
nano silver
silver
raw material
leaching solution
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Pending
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CN202110241811.0A
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Chinese (zh)
Inventor
方云
桂芳泽
游雨欣
陈芳容
洪慈清
潘晓鸿
关雄
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Fujian Agriculture and Forestry University
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Fujian Agriculture and Forestry University
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Priority to CN202110241811.0A priority Critical patent/CN113084182A/en
Publication of CN113084182A publication Critical patent/CN113084182A/en
Pending legal-status Critical Current

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/02—Making metallic powder or suspensions thereof using physical processes
    • B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
    • B22F2009/041—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by mechanical alloying, e.g. blending, milling

Abstract

The invention relates to a method for preparing nano-silver by taking tea leaching solution as a raw material, which comprises the following steps of: 1 tea leaf extract and 0.08mol/L AgNO3As a raw material for synthesizing nano-silver, tea leaching solution and AgNO are mixed by a plant reduction method3Placing the reaction solution mixed with the solution in a magnetic stirrer at 40 ℃ for stirring and reacting for 2 hours; centrifugally collecting the obtained nano silver, washing and drying the nano silver by using distilled water, and characterizing the particle size and the morphology of the obtained nano silver by using X-ray powder diffraction (XRD), a Scanning Electron Microscope (SEM) and a Zeta potential analyzer; the results show that the tea extract is used as the raw materialThe nano silver prepared by the material is in a small granular shape, the average size of the nano silver is 15.41nm, the potential is-13.91 +/-0.89 mV, and the average particle size of the nano silver in water is 773.49nm through calculation of a Sherle formula.

Description

Method for preparing nano-silver by using tea leaching solution as raw material
Technical Field
The invention belongs to the technical field of nano-silver preparation, and particularly relates to a method for preparing nano-silver by taking tea leaching solution as a raw material.
Background
The nano silver material has more excellent performances than common silver in various aspects such as physical chemistry and the like, such as unique electronic performance, optical performance, mechanical performance and catalytic performance, good antibacterial performance, biocompatibility performance, surface modification easiness and the like, is widely applied to the fields of chemical industry, medical treatment, biology and electronics, and has attracted wide attention at home and abroad in recent years.
The chemical reduction method is the most commonly used method for synthesizing nano silver at present, although the method can prepare stable nano silver with good dispersibility. However, the high temperature environment involved in the synthesis of nano silver increases energy consumption and cost. On the other hand, some reducing agents used in the synthesis of nano silver, such as ethylene glycol, sodium borohydride, pyridine, etc., may cause the generation of toxic substances, which may negatively affect the application of nano silver.
Based on this, the present application provides a method for preparing nano silver by using a plant reduction method, which can avoid the above disadvantages.
Disclosure of Invention
The invention aims to provide a method for preparing nano-silver by taking tea leaching solution as a raw material.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a method for preparing nano-silver by taking tea leaching solution as a raw material comprises the following steps:
1) extracting a tea leaching solution: adding weighed tea leaves into distilled water for soaking, then carrying out water bath at 90 ℃ for 30min, standing, cooling and carrying out suction filtration after the water bath is finished, collecting tea water, and removing tea residues in the tea water by using a filter to obtain a tea leaf extract;
2) preparing a nano-silver material by a plant reduction method: mixing the tea leaching solution prepared in the step 1) with AgNO3Mixing the solutions, and then carrying out stirring reaction at 40 ℃;
3) obtaining powdery nano silver: centrifuging the reaction product in the step 2), and taking the centrifugal precipitate and using ddH2And O, washing, centrifuging the washed precipitate, drying the precipitate obtained by centrifuging, and grinding the dried sample into fine powder in a mortar to obtain powdery nano silver.
Further, the adding amount of the tea leaves in the step 1) is 1.25g per hundred milliliters of the distilled water.
Preferably, the filter in step 1) is a 0.22 μm filter.
Further, AgNO in step 2)3The concentration of the solution is 0.08mol/L, wherein the tea extract and AgNO3The volume ratio of the solution is 1.5: 1, mixing.
Preferably, the rotation speed of the two centrifugal treatments in the step 3) is 10000r/min, and the centrifugal time is 20 min.
Preferably, the drying temperature of the precipitate in the step 3) is 50 ℃.
Preferably, the prepared nano silver has the particle size of 10-20 nm, the morphology is a more regular small granular structure with good dispersion, the Zeta potential is-13.91 +/-0.89 mV, and the average particle size in water is 773.49 nm.
The tea contains phytochemicals such as carboxylic acid, terpenoids, aldehydes, amides, flavones, ketones and the like, so that the nano-silver can be reduced. In addition, these phytochemicals can also interact with the surface of the nanoparticles, stabilizing the nanoparticles. The method for synthesizing the nano-silver by using the tea leaves is simple and cheap, and belongs to a green pollution-free synthesis method.
Compared with the prior art, the invention has the following beneficial effects:
1. the process of preparing the nano silver does not need high temperature, and can greatly reduce the energy consumption.
2. The invention only needs the tea leaching solution as a reducing agent, has simple raw material source, low price, environmental protection and high social and economic benefits.
Drawings
FIG. 1 is a photograph of the prepared nano-silver;
FIG. 2 is an X-ray powder diffraction analysis chart of the prepared nano silver;
FIG. 3 is the image of the prepared nano silver by scanning electron microscope.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
In the embodiment, oolong tea is selected as tea.
A tea leaf of commercially available oolong tea (6 g) was weighed, and soaked in 480ml of distilled water for 30min, followed by water bath at 90 ℃ for 30 min. After the water bath is finished, standing, cooling, performing suction filtration, collecting tea water, and removing tea residues in the tea water by using a 0.22 mu m filter to obtain a tea extract;
using tea extract and 0.08mol/L AgNO3The solution acts to generate precipitate to synthesize the nano silver. Weighing 450ml of tea extract and 300ml of 0.08mol/L AgNO3The solution is mixed and put into a magnetic stirrer with the temperature of 40 ℃ to be stirred and react for 2 h. Centrifuging at 10000r/min for 20min, collecting precipitate, and adding ddH2Washing with water for three times, centrifuging at 10000r/min for 20min, collecting precipitate, and oven drying at 50 deg.C. Grinding the dried sample into fine powder in a mortar, and storing the fine powder in a refrigerator at 4 ℃ for later use.
Example 2 characterization of the synthesized nanosilver
The size of the nano silver is calculated by adopting X-ray powder diffraction, and the appearance of the nano silver is observed by utilizing SEM. The result shows that the nano silver synthesized by the plant reduction method is completely consistent with the characteristic peak of a standard database card (JCPDF04-0783), the average size of the nano silver is about 15.41nm (figure 1) obtained by the Shele formula, and the synthesized nano silver has a small granular structure and certain agglomeration behavior (figure 2). The potential of the prepared nano silver measured by a Zeta potential analyzer is-13.91 +/-0.89 mV, and the data of DLS shows that the average particle size in water is 773.49 nm.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (7)

1. A method for preparing nano-silver by taking tea leaching solution as a raw material is characterized by comprising the following steps:
1) extracting a tea leaching solution: adding weighed tea leaves into distilled water for soaking, then carrying out water bath at 90 ℃ for 30min, standing, cooling and carrying out suction filtration after the water bath is finished, collecting tea water, and removing tea residues in the tea water by using a filter to obtain a tea leaf extract;
2) preparing a nano-silver material by a plant reduction method: mixing the tea leaching solution prepared in the step 1) with AgNO3Mixing the solutions, and then carrying out stirring reaction at 40 ℃;
3) obtaining powdery nano silver: centrifuging the reaction product in the step 2), and taking the centrifugal precipitate and using ddH2And O, washing, centrifuging the washed precipitate, drying the precipitate obtained by centrifuging, and grinding the dried sample into fine powder in a mortar to obtain powdery nano silver.
2. The method for preparing nano silver by using the tea extract as the raw material according to claim 1, wherein the amount of the tea leaves added in the step 1) is 1.25g per hundred milliliters of the distilled water.
3. The method for preparing nano silver from the tea leaching solution as the raw material according to claim 1, wherein the filter in the step 1) is a 0.22 μm filter.
4. The method for preparing nano silver by using tea leaching solution as raw material according to claim 2, wherein AgNO in the step 2)3The concentration of the solution is 0.08mol/L, wherein the tea extract and AgNO3The volume ratio of the solution is 1.5: 1, mixing.
5. The method for preparing nano silver from the tea leaching solution as the raw material according to claim 1, wherein the rotation speed of the two times of centrifugation in the step 3) is 10000r/min, and the centrifugation time is 20 min.
6. The method for preparing nano silver from the tea leaching solution as the raw material according to claim 1, wherein the drying temperature of the precipitate in the step 3) is 50 ℃.
7. The method for preparing nano silver by using the tea leaching solution as the raw material as claimed in claim 4, wherein the prepared nano silver has the particle size of 10-20 nm, the shape of the prepared nano silver is a regular small granular structure with good dispersion, the Zeta potential is-13.91 +/-0.89 mV, and the average particle size in water is 773.49 nm.
CN202110241811.0A 2021-03-04 2021-03-04 Method for preparing nano-silver by using tea leaching solution as raw material Pending CN113084182A (en)

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Publication number Priority date Publication date Assignee Title
KR20060033283A (en) * 2004-10-14 2006-04-19 주식회사 국일인토트 Composition containing nano-particle of silver
CN102202815A (en) * 2008-05-16 2011-09-28 维鲁泰克技术股份有限公司 Green synthesis of nanometals using plant extracts and use thereof
CN104923805A (en) * 2015-07-03 2015-09-23 渤海大学 Micro-nano-silver base material preparation method and micro-nano-silver base material thereof
CN105665737A (en) * 2016-01-27 2016-06-15 陕西科技大学 Biosynthesis method of nano Ag
CN107186223A (en) * 2017-05-22 2017-09-22 上海理工大学 A kind of method that utilization China pink tea leaching liquor prepares silver nano-grain
CN107363269A (en) * 2017-09-23 2017-11-21 信阳师范学院 A kind of preparation method of the Nano silver solution based on tea powder
US20180027821A1 (en) * 2016-08-01 2018-02-01 Je Shu Cho Method for preparing sterilizing deodorant and sterilizing deodorant prepared thereby

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20060033283A (en) * 2004-10-14 2006-04-19 주식회사 국일인토트 Composition containing nano-particle of silver
CN102202815A (en) * 2008-05-16 2011-09-28 维鲁泰克技术股份有限公司 Green synthesis of nanometals using plant extracts and use thereof
CN104923805A (en) * 2015-07-03 2015-09-23 渤海大学 Micro-nano-silver base material preparation method and micro-nano-silver base material thereof
CN105665737A (en) * 2016-01-27 2016-06-15 陕西科技大学 Biosynthesis method of nano Ag
US20180027821A1 (en) * 2016-08-01 2018-02-01 Je Shu Cho Method for preparing sterilizing deodorant and sterilizing deodorant prepared thereby
CN107186223A (en) * 2017-05-22 2017-09-22 上海理工大学 A kind of method that utilization China pink tea leaching liquor prepares silver nano-grain
CN107363269A (en) * 2017-09-23 2017-11-21 信阳师范学院 A kind of preparation method of the Nano silver solution based on tea powder

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Application publication date: 20210709