CN113714508A - Nano silver and preparation method and application thereof - Google Patents
Nano silver and preparation method and application thereof Download PDFInfo
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 25
- 229910052709 silver Inorganic materials 0.000 claims abstract description 22
- 239000004332 silver Substances 0.000 claims abstract description 22
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 19
- 239000003223 protective agent Substances 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000002156 mixing Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical group OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- 239000002244 precipitate Substances 0.000 claims description 11
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 10
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 10
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 9
- 239000012498 ultrapure water Substances 0.000 claims description 9
- 230000000844 anti-bacterial effect Effects 0.000 claims description 8
- 239000002211 L-ascorbic acid Substances 0.000 claims description 7
- 235000000069 L-ascorbic acid Nutrition 0.000 claims description 7
- 229960005070 ascorbic acid Drugs 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 3
- 239000002671 adjuvant Substances 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 40
- 239000013078 crystal Substances 0.000 abstract description 9
- 230000035484 reaction time Effects 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 7
- 239000007769 metal material Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- 238000002441 X-ray diffraction Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000009826 distribution Methods 0.000 description 7
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 238000005054 agglomeration Methods 0.000 description 5
- 230000002776 aggregation Effects 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 238000002425 crystallisation Methods 0.000 description 4
- 230000008025 crystallization Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000010899 nucleation Methods 0.000 description 4
- 230000006911 nucleation Effects 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 231100000614 poison Toxicity 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000003440 toxic substance Substances 0.000 description 2
- 230000005653 Brownian motion process Effects 0.000 description 1
- -1 adopts three methods Chemical compound 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 238000005537 brownian motion Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000003745 diagnosis Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001415 gene therapy Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 230000005476 size effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
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Abstract
本发明涉及一种纳米银及其制备方法和应用，属于纳米金属材料技术领域。所述纳米银的制备方法为：将银源、保护剂及还原剂混合于水中，形成混合溶液；将所述混合溶液进行超声处理，同时进行微波加热至20～80℃反应5～20min，得到纳米银。本发明制得的纳米银结晶度高、粒径小而均匀，且本发明合成工艺高效、简便、环保，原料易得，重现性好，有效解决了传统化学法反应时间长，产物晶型不完整，容易团聚，反应体系不环保等问题。
The invention relates to a kind of nanometer silver, a preparation method and application thereof, and belongs to the technical field of nanometer metal materials. The preparation method of the nano-silver is as follows: mixing a silver source, a protective agent and a reducing agent in water to form a mixed solution; subjecting the mixed solution to ultrasonic treatment, and simultaneously heating the mixed solution to 20-80 DEG C for 5-20 minutes, to obtain Nano silver. The nano-silver prepared by the invention has high crystallinity, small and uniform particle size, and the synthesis process of the invention is efficient, simple and environmentally friendly, the raw materials are easily available, and the reproducibility is good, and the traditional chemical method effectively solves the problem of long reaction time and product crystal form. Incomplete, easy to agglomerate, and the reaction system is not environmentally friendly.
Description
Technical Field
The invention relates to the technical field of nano metal materials, in particular to nano silver and a preparation method and application thereof.
Background
The nano silver has volume effect, surface effect, quantum size effect and macroscopic quantum tunneling effect, has special properties in optical, electronic, thermal and biomedical materials, and also has magnetism and excellent antibacterial performance. Has wide application prospect in the fields of industrial catalytic materials, electronic components, antistatic materials, low-temperature superconducting materials, antibacterial materials, molecular diagnosis, gene therapy and the like. Especially as a catalyst, the catalyst has better catalytic activity and reaction selectivity. Because of the wide application of nano-silver in various fields such as medical treatment, catalysis, antibacterial activity and the like, it is necessary to adopt a low-toxicity or even non-toxic method to prepare the nano-silver which is harmless to human bodies and is environment-friendly. Based on the consideration of the aspects of economy, environmental protection, large-scale production and the like, the method for preparing the nano silver particles by finding an efficient, simple and harmless synthesis method has important significance.
At present, the domestic preparation method of nano-silver mainly adopts three methods, namely a physical method, a chemical method and a biological method. The chemical method for preparing the nano silver particles is common, the method is simple to operate and easy to control, but the method has the defects of long reaction time, incomplete crystal form of the product, easy agglomeration of product particles, general preparation reaction in an organic solvent and no environmental protection of a reaction system.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide nano silver and a preparation method and application thereof, and aims to solve the problems that the existing preparation method is long in reaction time and the crystal form of the prepared nano silver particles is incomplete.
The invention adopts the following technical scheme:
a preparation method of nano silver comprises the following steps:
mixing a silver source, a protective agent and a reducing agent in water to form a mixed solution;
and carrying out ultrasonic treatment on the mixed solution, and simultaneously carrying out microwave heating to 20-80 ℃ for reaction for 5-20 min to obtain the nano silver.
Optionally, the silver source is silver nitrate.
Optionally, the protectant is sodium dodecylbenzenesulfonate.
Optionally, the reducing agent is L-ascorbic acid.
Optionally, the molar ratio of the silver source to the protective agent is 1: 1-5: 1.
optionally, the molar ratio of the silver source to the reducing agent is 1: 3-1: 6.
optionally, the preparation method further comprises the steps of: and cooling the solution after the reaction, performing suction filtration, washing and drying the precipitate obtained by suction filtration to obtain the nano-silver.
Optionally, the water is ultrapure water.
The nano silver prepared by the preparation method of the nano silver is provided.
The application of the nano-silver prepared by the preparation method of the nano-silver in the invention in antibacterial auxiliary materials.
Compared with the prior art, the invention has the following beneficial effects: the nano silver is obtained by uniformly dispersing with the assistance of ultrasonic waves and reacting for 5-20 min after microwave heating to 20-80 ℃. Namely, the method adopts the ultrasonic microwave to assist the chemical reduction method to prepare the powdery nano silver, integrates the advantages of the ultrasonic microwave and the chemical reduction method, is efficient, simple and environment-friendly, obtains the nano silver powder with high crystallinity, small and uniform particle size, and can be better applied to the fields of nano silver antibacterial auxiliary materials and the like. The method effectively solves the problems of long reaction time, incomplete crystal form of the prepared silver nanoparticles, nanoparticle agglomeration and introduction of toxic substances in the existing preparation method.
Drawings
FIG. 1 is an X-ray diffraction pattern of a sample of example 1;
FIG. 2 is a SEM photograph of a sample of example 1;
FIG. 3 shows the UV-Vis spectrometer test results of the sample of example 1;
FIG. 4 is an X-ray diffraction pattern of a sample of example 2;
FIG. 5 is a SEM photograph of a sample of example 2;
FIG. 6 shows the UV-Vis spectrometer test results of the sample of example 2;
FIG. 7 is an X-ray diffraction pattern of a sample of example 3;
FIG. 8 is a SEM photograph of a sample of example 3;
FIG. 9 shows the UV-Vis spectrometer test results of the sample of example 3;
FIG. 10 is an X-ray diffraction pattern of a sample of example 4;
FIG. 11 is a SEM photograph of a sample of example 4;
FIG. 12 shows the UV-Vis spectrometer test results of the sample of example 4.
Detailed Description
The present invention is described in further detail below by way of specific embodiments, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention.
The embodiment of the invention provides a preparation method of nano silver, which comprises the following steps:
mixing a silver source, a protective agent and a reducing agent in water to form a mixed solution;
and carrying out ultrasonic treatment on the mixed solution, and simultaneously carrying out microwave heating to 20-80 ℃ for reaction for 5-20 min to obtain the nano silver.
In the embodiment, the nano-silver is obtained by uniformly dispersing with the aid of ultrasonic wave and simultaneously heating the mixture to 20-80 ℃ by microwave for reaction for 5-20 min. Namely, the method adopts the ultrasonic microwave to assist the chemical reduction method to prepare the powdery nano silver, integrates the advantages of the ultrasonic microwave and the chemical reduction method, is efficient, simple and environment-friendly, obtains the nano silver powder with high crystallinity, small and uniform particle size, and can be better applied to the fields of nano silver antibacterial auxiliary materials and the like. The method effectively solves the problems of long reaction time, incomplete crystal form of the prepared silver nanoparticles, nanoparticle agglomeration and introduction of toxic substances in the existing preparation method.
Preferably, the particle size of the nano silver is 50-100 nm.
Preferably, the microwave is heated to 20-60 ℃ to further ensure that the particle size of the prepared nano silver is small.
Preferably, the microwave is heated to 20-80 ℃ for reaction for 10-20 min, such as 20min, so as to further ensure that the particle size of the prepared nano silver is small.
Preferably, the silver source is silver nitrate.
Preferably, the protective agent is sodium dodecyl benzene sulfonate.
Preferably, the reducing agent is L-ascorbic acid.
Preferably, the molar ratio of the silver source to the protective agent is 1: 1-5: 1. the appropriate amount of the protective agent can promote the nucleation of the nano silver particles, so that the prepared nano silver has smaller particle size, and the excessive protective agent can cause the nano silver particles to grow up.
Preferably, the molar ratio of the silver source to the reducing agent is 1: 3-1: 6. the nano silver particles with smaller particle size can be obtained by using a proper amount of the reducing agent, and the particle size and the distribution of the nano silver particles are influenced by improper amount of the reducing agent.
Optionally, the preparation method further comprises the steps of: and cooling the solution after the reaction, performing suction filtration, washing and drying the precipitate obtained by suction filtration to obtain the nano-silver.
Optionally, the water is ultrapure water.
The nano silver is prepared by the preparation method of the nano silver provided by the embodiment of the invention.
The application of the nano-silver prepared by the preparation method of the nano-silver provided by the embodiment of the invention in antibacterial auxiliary materials.
The invention is further illustrated by the following specific examples.
Example 1
Weighing 0.51g of silver nitrate, 0.5g of sodium dodecyl benzene sulfonate and 3.17g L-ascorbic acid, respectively dissolving in 5mL, 10mL and 15mL of ultrapure water, and mixing to form a mixed solution; uniformly dispersing by ultrasonic assistance, and simultaneously heating to 20 deg.C, 40 deg.C, 60 deg.C, and 80 deg.C with microwave respectively, reacting for 20min respectively until precipitate is completely generated, cooling, vacuum filtering, washing precipitate, and drying to obtain powdered nano silver.
The obtained nano silver is characterized by adopting an X-ray diffractometer, a field emission scanning electron microscope and an ultraviolet visible spectrophotometer.
Fig. 1 is an X-ray diffraction spectrum of the nano-silver obtained in this example, fig. 2 is a scanning electron microscope photograph of the nano-silver obtained in this example, and fig. 3 is a test result of the uv-vis spectrometer of the nano-silver obtained in this example.
As can be seen from figure 1, the XRD diffraction peak of the obtained sample is consistent with the diffraction peak of a silver standard card (Ag JCPDS No.04-0783), all main diffraction peaks are obviously separated, all the diffraction peaks are sharp and clear, and the peak shape and peak height reach the standard, so that the powder crystallization is relatively complete, and the sample is a high-crystallinity silver simple substance and belongs to a face-centered cubic crystal structure. The average particle size of the nano silver is about 50 nm by fitting each peak and estimating by using the scherrer equation d ═ k λ/BCos θ. As can be seen from FIG. 2, the obtained silver nanoparticles are spherical, and have uniform dispersion and obvious agglomeration at 80 ℃. As can be seen from FIG. 3, the maximum absorption peak is first blue-shifted and then red-shifted with increasing temperature. This shows that the particle size of the nano silver is increased after being reduced with the increase of the temperature, and the half-peak width of the absorption spectrum is widest when the temperature is 80 ℃, which shows that the particle size distribution of the nano silver prepared under the condition is widest. This demonstrates that increasing the temperature at 20 ℃ to 60 ℃ is beneficial in increasing the nucleation rate; when the temperature reaches 80 ℃, the Brownian motion is accelerated by the overhigh temperature, and the agglomeration of the nano silver is accelerated, so that the particle size distribution is wider.
Example 2
Weighing 0.51g of silver nitrate, 0.5g of sodium dodecyl benzene sulfonate and 3.17g L-ascorbic acid, respectively dissolving in 5mL, 10mL and 15mL of ultrapure water, and mixing to form a mixed solution; uniformly dispersing by ultrasonic assistance, heating to 20 deg.C with microwave, reacting for 5min, 10min, 15min, and 20min respectively until precipitate is completely generated, cooling, vacuum filtering, washing the precipitate, and drying to obtain powdered nano silver.
The obtained nano silver is characterized by adopting an X-ray diffractometer, a field emission scanning electron microscope and an ultraviolet visible spectrophotometer.
Fig. 4 is an X-ray diffraction spectrum of the nano-silver obtained in this embodiment, fig. 5 is a scanning electron microscope photograph of the nano-silver obtained in this embodiment, and fig. 6 is a test result of the uv-vis spectrometer of the nano-silver obtained in this embodiment.
As can be seen from FIG. 4, the XRD diffraction peak of the obtained sample is consistent with the diffraction peak of a silver standard card (Ag JCPDS No.04-0783), all main diffraction peaks are obviously separated, all the diffraction peaks are sharp and clear, and the peak shape and peak height reach the standard, which indicates that the powder is more complete in crystallization, and indicates that the sample is a high-crystallinity silver simple substance and belongs to a face-centered cubic crystal structure. The average particle size of the nano silver is about 50 nm by fitting each peak and estimating by using the scherrer equation d ═ k λ/BCos θ. As can be seen from fig. 5, the obtained silver nanoparticles are spherical and relatively uniformly dispersed. As can be seen from fig. 6, as the reaction time increases, the maximum absorption peak wavelength is shortest when the time is 20min, which indicates that the particle size of the nano-silver is smallest under this condition, and the half-peak width of the absorption spectrum is widest when the time is 5min, which indicates that the particle size distribution of the nano-silver particles is widest under this condition, which indicates that too short reaction time affects the nucleation of the nano-silver particles, resulting in broadening of the particle size distribution.
Example 3
Weighing 0.51g of silver nitrate, 0.1g of sodium dodecyl benzene sulfonate, 0.2g of sodium dodecyl benzene sulfonate, 0.3g of sodium dodecyl benzene sulfonate, 0.4g of sodium dodecyl benzene sulfonate and 3.17g of L-ascorbic acid, respectively dissolving in 5mL of ultrapure water, 10mL of ultrapure water and 15mL of ultrapure water, and mixing to form a mixed solution; uniformly dispersing by ultrasonic assistance, simultaneously heating to 20 ℃ by microwave, reacting for 20min until the generated precipitate is complete, cooling, filtering, washing the precipitate, and drying to obtain powdery nano silver.
The obtained nano silver is characterized by adopting an X-ray diffractometer, a field emission scanning electron microscope and an ultraviolet visible spectrophotometer.
Fig. 7 is an X-ray diffraction spectrum of the nano-silver obtained in this example, fig. 8 is a scanning electron micrograph of the nano-silver obtained in this example, and fig. 9 is a test result of the uv-vis spectrometer of the nano-silver obtained in this example.
As can be seen from FIG. 7, the XRD diffraction peak of the obtained sample is consistent with the diffraction peak of a silver standard card (Ag JCPDS No.04-0783), all main diffraction peaks are obviously separated, all the diffraction peaks are sharp and clear, and the peak shape and peak height reach the standard, which indicates that the powder is more complete in crystallization, and indicates that the sample is a high-crystallinity silver simple substance and belongs to a face-centered cubic crystal structure. The average particle size of the nano silver is about 50 nm by fitting each peak and estimating by using the scherrer equation d ═ k λ/BCos θ. As can be seen from fig. 8, the obtained silver nanoparticles were spherical and relatively uniformly dispersed. As can be seen from fig. 9, increasing the amount of the protecting agent can red-shift the maximum absorption peak, i.e. the size of the nano-silver particles under this condition increases with the amount of the protecting agent, i.e. a proper amount of the protecting agent can promote the nucleation of the nano-silver particles, and an excessive amount of the protecting agent can cause the nano-silver particles to grow up.
Example 4
Weighing 0.51g of silver nitrate, 0.5g of sodium dodecyl benzene sulfonate and 1.58g, 2.11g, 2.64g and 3.17g L-ascorbic acid, respectively dissolving in 5mL, 10mL and 15mL of ultrapure water, and mixing to form a mixed solution; uniformly dispersing by ultrasonic assistance, simultaneously heating to 20 ℃ by microwave, reacting for 20min until the generated precipitate is complete, cooling, filtering, washing the precipitate, and drying to obtain powdery nano silver.
The obtained nano silver is characterized by adopting an X-ray diffractometer, a field emission scanning electron microscope and an ultraviolet visible spectrophotometer.
Fig. 10 is an X-ray diffraction spectrum of the nano-silver obtained in this example, fig. 11 is a scanning electron micrograph of the nano-silver obtained in this example, and fig. 12 is a test result of the uv-vis spectrometer of the nano-silver obtained in this example.
As can be seen from FIG. 10, the XRD diffraction peak of the obtained sample is consistent with that of a silver standard card (Ag JCPDS No.04-0783), all main diffraction peaks are obviously separated, all the diffraction peaks are sharp and clear, and the peak shape and peak height reach the standard, so that the powder crystallization is relatively complete, and the sample is a high-crystallinity silver simple substance and belongs to a face-centered cubic crystal structure. The average particle size of the nano silver is about 50 nm by fitting each peak and estimating by using the scherrer equation d ═ k λ/BCos θ. As can be seen from fig. 11, the obtained silver nanoparticles were spherical and relatively uniformly dispersed. As can be seen from fig. 12, the maximum absorption peak of the sample is first blue-shifted and then red-shifted with increasing amount of the reducing agent, indicating that the particle size is first decreased and then increased. When the nano silver particles have the smallest particle size, the smallest half-peak width and the narrowest particle size distribution, the Vc dosage is 2.11 g. Namely, the nano silver particles with smaller particle size can be obtained by using a proper amount of the reducing agent, and the particle size and the distribution of the nano silver particles are affected by improper amount of the reducing agent.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of protection is not limited thereto. The equivalents and modifications of the present invention which may occur to those skilled in the art are within the scope of the present invention as defined by the appended claims.
Claims (10)
1. A preparation method of nano silver is characterized by comprising the following steps:
mixing a silver source, a protective agent and a reducing agent in water to form a mixed solution;
and carrying out ultrasonic treatment on the mixed solution, and simultaneously carrying out microwave heating to 20-80 ℃ for reaction for 5-20 min to obtain the nano silver.
2. The method for preparing nano silver according to claim 1, wherein the silver source is silver nitrate.
3. The method for preparing nano silver according to claim 1, wherein the protective agent is sodium dodecyl benzene sulfonate.
4. The method for preparing nano silver according to claim 1, wherein the reducing agent is L-ascorbic acid.
5. The method for preparing nano silver according to claim 1, wherein the molar ratio of the silver source to the protective agent is 1: 1-5: 1.
6. the method for preparing nano silver according to claim 1, wherein the molar ratio of the silver source to the reducing agent is 1: 3-1: 6.
7. the method for preparing nano silver according to claim 1, further comprising the steps of: and cooling the solution after the reaction, performing suction filtration, washing and drying the precipitate obtained by suction filtration to obtain the nano-silver.
8. The method of claim 1, wherein the water is ultrapure water.
9. Nano silver produced by the method for producing nano silver according to any one of claims 1 to 8.
10. Use of nano silver prepared by the method of any one of claims 1 to 8 in antibacterial adjuvants.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117259772A (en) * | 2023-08-25 | 2023-12-22 | 江苏农林职业技术学院 | Radix puerariae nano-silver composite hydrosol and preparation method and application thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040147618A1 (en) * | 2001-04-30 | 2004-07-29 | Lee Mu Sang | Colloid solution of metal nanoparticles, metal-polymer nanocomposites and methods for preparation thereof |
| JP2008106315A (en) * | 2006-10-26 | 2008-05-08 | National Institute Of Advanced Industrial & Technology | Metal nanoparticles and method for producing the same |
| CN102101173A (en) * | 2009-12-22 | 2011-06-22 | 上海亿金纳米科技有限公司 | Method for preparing novel large-scale oil-soluble nano silver |
| CN102923760A (en) * | 2012-12-02 | 2013-02-13 | 桂林理工大学 | Ultrasonic/microwave synergistic constant-pressure solvothermal synthesis method of cubic-structure and hexagonal-structure nano ZnS semiconductor material |
| CN111496269A (en) * | 2020-05-21 | 2020-08-07 | 广州大学附属中学 | Nano silver and preparation method and application thereof |
| CN112828300A (en) * | 2020-12-28 | 2021-05-25 | 长沙新材料产业研究院有限公司 | Nano silver, preparation method and application |
-
2021
- 2021-08-12 CN CN202110925764.1A patent/CN113714508A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040147618A1 (en) * | 2001-04-30 | 2004-07-29 | Lee Mu Sang | Colloid solution of metal nanoparticles, metal-polymer nanocomposites and methods for preparation thereof |
| JP2008106315A (en) * | 2006-10-26 | 2008-05-08 | National Institute Of Advanced Industrial & Technology | Metal nanoparticles and method for producing the same |
| CN102101173A (en) * | 2009-12-22 | 2011-06-22 | 上海亿金纳米科技有限公司 | Method for preparing novel large-scale oil-soluble nano silver |
| CN102923760A (en) * | 2012-12-02 | 2013-02-13 | 桂林理工大学 | Ultrasonic/microwave synergistic constant-pressure solvothermal synthesis method of cubic-structure and hexagonal-structure nano ZnS semiconductor material |
| CN111496269A (en) * | 2020-05-21 | 2020-08-07 | 广州大学附属中学 | Nano silver and preparation method and application thereof |
| CN112828300A (en) * | 2020-12-28 | 2021-05-25 | 长沙新材料产业研究院有限公司 | Nano silver, preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 周惠久: "新材料词典", 31 December 1996, 上海科学技术文献出版社, pages: 583 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117259772A (en) * | 2023-08-25 | 2023-12-22 | 江苏农林职业技术学院 | Radix puerariae nano-silver composite hydrosol and preparation method and application thereof |
| CN117259772B (en) * | 2023-08-25 | 2024-05-10 | 江苏农林职业技术学院 | A kudzu root nano-silver composite hydrosol and its preparation method and application |
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