CN114160785B - Preparation method of mild condition controllable nano silver solution - Google Patents
Preparation method of mild condition controllable nano silver solution Download PDFInfo
- Publication number
- CN114160785B CN114160785B CN202111361819.7A CN202111361819A CN114160785B CN 114160785 B CN114160785 B CN 114160785B CN 202111361819 A CN202111361819 A CN 202111361819A CN 114160785 B CN114160785 B CN 114160785B
- Authority
- CN
- China
- Prior art keywords
- nano silver
- mol
- particle size
- silver solution
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 40
- 239000002245 particle Substances 0.000 claims abstract description 31
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 22
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 22
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 20
- 239000001509 sodium citrate Substances 0.000 claims abstract description 18
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims abstract description 18
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 16
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 16
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 16
- 239000012498 ultrapure water Substances 0.000 claims abstract description 16
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000003223 protective agent Substances 0.000 claims abstract description 7
- 239000002270 dispersing agent Substances 0.000 claims abstract description 6
- 229910052709 silver Inorganic materials 0.000 claims abstract description 6
- 239000004332 silver Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 22
- 229960005070 ascorbic acid Drugs 0.000 claims description 15
- 235000010323 ascorbic acid Nutrition 0.000 claims description 15
- 239000011668 ascorbic acid Substances 0.000 claims description 15
- 238000009826 distribution Methods 0.000 abstract description 8
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 238000005054 agglomeration Methods 0.000 abstract description 3
- 238000011031 large-scale manufacturing process Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000008103 glucose Substances 0.000 description 6
- 239000012279 sodium borohydride Substances 0.000 description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 description 6
- 230000000844 anti-bacterial effect Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000003917 TEM image Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000008014 freezing Effects 0.000 description 2
- 238000007710 freezing Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000004659 sterilization and disinfection Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 230000029663 wound healing Effects 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 108010039918 Polylysine Proteins 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000010261 cell growth Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000012567 medical material Substances 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 229920000656 polylysine Polymers 0.000 description 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000014599 transmission of virus Effects 0.000 description 1
- 230000005641 tunneling Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- 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
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
-
- 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
Abstract
The invention discloses a room temperature and condition controllable particle size nano silver solution, which is prepared by taking ultrapure water as a solvent, silver nitrate as a silver source, sodium citrate as a protective agent, polyvinylpyrrolidone as a dispersing agent and a reducing agent with a certain concentration under the action of the reducing agent, and has good dispersibility, sphericity and anti-agglomeration nano silver solution with the particle size of about 60 nm. The nano silver solution has good dispersibility, controllable particle size distribution and spherical nano silver shape. The invention designs a preparation method of the nano silver solution with low requirements on equipment, simple process, mild reaction conditions, simple and convenient operation, suitability for large-scale production and good product performance.
Description
Technical Field
The invention belongs to the technical field of new nano materials, and particularly relates to a preparation method of a nano silver solution with controllable room temperature and temperature conditions.
Background
The nano technology is the most promising new technology in the 21 st century, combines the biological principle with the physical and chemical processes to generate nano particles with specific functions, is widely applied to the fields of information, biology, medicine, chemical industry, aerospace, energy sources, national defense and the like, and has huge market potential. In recent years, metal nanoparticles have received attention because of their unique magnetic, electronic configuration, optical, and other properties. The nano silver material has very stable physical and chemical properties, has very excellent properties in various aspects such as electricity, optics and catalysis, and is widely applied to various fields such as biological medicine, ceramic materials, environment-friendly materials, paint and the like. More importantly, the extremely small amount of nano silver can generate strong bactericidal effect, broad-spectrum sterilization and no drug resistance, can promote wound healing, cell growth and damaged cell repair, has no toxic reaction, and has no stimulation reaction to skin, thus opening up a wide prospect for widely applying nano silver for antibacterial.
The particle size of nano silver is distributed between 1-100 nm, the atomic arrangement is in a 'medium state' between solid and molecule, the specific surface area is large, the surface effect, the small-size effect and the macroscopic quantum tunneling effect are provided, the surface activity is enhanced, and the nano silver has strong penetrating power and antibacterial capability. Therefore, the nano silver solution with controllable particle size can be applied to daily life, such as masks, clothes and the like, and plays a role in strong sterilization and disinfection.
AgNPs are synthesized by sol-gel method, solvent-thermal synthesis method, chemical reduction method, laser ablation method, inert gas condensation method and other different physical and chemical methods, the principle of the physical method is simple, the obtained product has few impurities and good quality, but has higher requirements on instruments and equipment and high production cost. The chemical method is simpler, but has higher requirements on controlling the particle size, and the particle size is controlled by variable factors with different conditions.
Chinese patent 201010148262.4 discloses a preparation method of water-soluble nano silver, wherein silver salt and a protective agent are stirred and dissolved in water at 30-60 ℃, the pH value is regulated, when a solution system is clear and transparent for 5-20 minutes, a reducing agent is added into a reaction system, and then stirring and reacting are continued for 5-30 minutes.
Chinese patent 201410344102.5 discloses a preparation method of nano silver sol, which comprises the steps of mixing silver nitrate solution or silver ammonia solution with polylysine water solution, stirring and reacting for 30-180 minutes at 500-100 ℃ to obtain nano silver sol.
Chinese patent 201410850968.3 discloses a method for preparing and preserving colorless nano silver sol by using low temperature technology, which adopts the steps of dissolving silver source in water, uniformly mixing, freezing and crushing to obtain the ice sand containing silver raw material. And then dissolving the reducing agent in water, uniformly mixing, freezing and crushing to obtain the ice sand containing the reducing agent. And mixing the obtained ice sand containing the silver raw material with the ice sand containing the reducing agent, and grinding to obtain the nano silver ice crystals.
Said invention requires the regulation of temperature and pH value in specific range, and is not suitable for large-scale industrial production.
Disclosure of Invention
Aiming at the problems in the background technology, the invention provides the preparation method of the nano silver solution, which has low requirements on equipment, simple process, mild reaction conditions, simple and convenient operation, suitability for large-scale production and good product performance.
The technical scheme adopted for solving the technical problems is as follows: a method for preparing a mild condition controllable nano silver solution, which takes ultrapure water as a solvent, takes high-grade pure silver nitrate with the content of 99.95 percent as a silver source, takes Sodium Citrate (TSC) as a protective agent, takes polyvinylpyrrolidone (PVP, K30) as a dispersing agent, takes ascorbic acid, glucose or sodium borohydride as a reducing agent, sequentially adds 50 mu L of silver nitrate with the concentration of 0.05mol/L, 0.8 mL of sodium citrate (TSC) with the concentration of 0.075mol/L and 0.3-1.0 mL of polyvinylpyrrolidone (PVP, K30) with the concentration of 0.3-1.0 mL mol/L into 50mL of ultrapure water at room temperature, and after a solution system is stirred for 3min at the rotating speed of 400r/min, 0.2-0.5 mL of the reducing agent with the concentration of 0.1mol/L is added into a reaction system, and then continuously stirred for 30min, so that a nano silver solution with good dispersibility and anti-agglomeration performance, the particle size of about 60nm, the nano silver solution with good dispersibility and controllable particle size distribution, and nano silver shape, is spherical, is prepared.
Further, the molar ratio of sodium citrate (TSC) to silver nitrate is 9-24:1.
Further, the molar ratio of polyvinylpyrrolidone (PVP, K30) to silver nitrate is 2.1-7:1.
Further, the molar ratio of the reducing agent to the silver nitrate is 8-20:1.
The beneficial effects of the invention are as follows:
the system researches the reduction effect and mechanism of reducing agents such as sodium borohydride, glucose, ascorbic acid and the like on silver nitrate, controls the nucleation size, shape and speed of nano silver by adjusting the types and dosage of the reducing agents, and the obtained nano silver solution has high stable dispersion performance, no obvious agglomeration sedimentation phenomenon in three months, the average particle size of nano silver is about 60nm, and the prepared concentration is diluted by ultrapure water so as to prevent the influence of water ions.
The invention has low preparation cost, low energy consumption, no toxic and harmful waste, and meets the requirement of green production. The method has the advantages of low requirements on equipment, simple process, mild reaction conditions, simple and convenient operation, suitability for large-scale production and good product performance.
The preparation process is simple, the particle size and the morphology of the nano silver particles can be accurately regulated and controlled, the product can be used for antibacterial medical materials such as wound healing, antibacterial textiles and footwear, and can act on a mask to effectively inhibit the transmission of viruses.
Drawings
FIG. 1 is a TEM image of a nanosilver solution of the invention (TSC 0.3-0.8 mL (0.075 mol/L));
FIG. 2 is a TEM image of a nanosilver solution of the invention (ascorbic acid 0.5mL (0.1 mol/L));
FIG. 3 is a graph showing the particle size distribution of the nano-silver solution prepared by the present invention.
Detailed Description
The following description of the embodiments of the invention is presented in conjunction with the accompanying drawings to provide a better understanding of the invention to those skilled in the art. It is to be expressly noted that in the description below, detailed descriptions of known functions and designs are omitted here as perhaps obscuring the present invention.
The invention discloses a preparation method of a mild condition controllable nano silver solution, which comprises the steps of sequentially adding 50 mu L (0.05 mol/L) of silver nitrate, 0.3-0.8 mL (0.075 mol/L) of sodium citrate (TSC) and 0.3-1.0 mL (0.0175 mol/L) of polyvinylpyrrolidone into 50mL of ultrapure water, rapidly stirring at the rotating speed of 400r/min, dispersing uniformly, adding 0.2-0.5 mL (0.1 mol/L) of ascorbic acid, 0.2mL (0.1 mol/L) of sodium borohydride or 0.2mL (0.1M) of glucose after 3 minutes, and continuously stirring for 30 minutes.
Examples 1 to 8 the amounts of the test materials added are shown in the following table.
Example 1
A preparation method of a mild condition controllable nano silver solution comprises the steps of sequentially adding 50 mu L (0.05 mol/L) of silver nitrate, 0.3 mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone into 50mL of ultrapure water, rapidly stirring at a rotating speed of 400r/min, dispersing uniformly, adding 0.2mL (0.1 mol/L) of ascorbic acid after 3 minutes, and continuously stirring for 30 minutes.
Example 2
A preparation method of a mild condition controllable nano silver solution comprises the steps of sequentially adding 50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone into 50mL of ultrapure water, rapidly stirring at a rotating speed of 400r/min, dispersing uniformly, adding 0.2mL (0.1 mol/L) of ascorbic acid after 3 minutes, and continuously stirring for 30 minutes.
Example 3
A preparation method of a mild condition controllable nano silver solution comprises the steps of sequentially adding 50 mu L (0.05 mol/L) of silver nitrate, 0.8 mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone into 50mL of ultrapure water, rapidly stirring at a rotating speed of 400r/min, dispersing uniformly, adding 0.2mL (0.1 mol/L) of ascorbic acid after 3 minutes, and continuously stirring for 30 minutes.
Example 4
A preparation method of a mild condition controllable nano silver solution comprises the steps of sequentially adding 50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.3 mL (0.0175 mol/L) of polyvinylpyrrolidone into 50mL of ultrapure water, rapidly stirring at a rotating speed of 400r/min, dispersing uniformly, adding 0.2mL (0.1 mol/L) of ascorbic acid after 3 minutes, and continuously stirring for 30 minutes.
Example 5
A preparation method of a mild condition controllable nano silver solution comprises the steps of sequentially adding 50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 1.0 mL (0.0175 mol/L) of polyvinylpyrrolidone into 50mL of ultrapure water, rapidly stirring at a rotating speed of 400r/min, dispersing uniformly, adding 0.2mL (0.1 mol/L) of ascorbic acid after 3 minutes, and continuously stirring for 30 minutes.
Example 6
A preparation method of a mild condition controllable nano silver solution comprises the steps of sequentially adding 50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone into 50mL of ultrapure water, rapidly stirring at a rotating speed of 400r/min, dispersing uniformly, adding 0.5mL (0.1 mol/L) of ascorbic acid after 3 minutes, and continuously stirring for 30 minutes.
Example 7
A preparation method of a mild condition controllable nano silver solution comprises the steps of sequentially adding 50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone into 50mL of ultrapure water, rapidly stirring at a rotating speed of 400r/min, dispersing uniformly, adding 0.2mL (0.1 mol/L) of sodium borohydride after 3 minutes, and continuously stirring for 30 minutes.
Example 8
A preparation method of a mild condition controllable nano silver solution comprises the steps of sequentially adding 50 mu L (0.05 mol/L) of silver nitrate, 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone into 50mL of ultrapure water, rapidly stirring at a rotating speed of 400r/min, dispersing uniformly, adding 0.2mL (0.1 mol/L) of glucose after 3 minutes, and continuously stirring for 30 minutes.
Examples 1-8 nanosilver solutions have particle size distribution, average particle size and polydispersity index test results as shown in the following table:
in examples 1, 2 and 3, sodium citrate (TSC) (0.075 mol/L) is used as a variable, the effect of the protecting agent TSC is obvious, the particle size gradually decreases along with the increase of the volume of the TSC solution, but after the TSC reaches a certain volume, the dispersibility is poor along with the increase of the volume of the TSC solution, the particle size has a small increasing trend, and the aggregation phenomenon of nano silver particles is obvious. From the TEM image of FIG. 1, it can be seen that the protecting agent TSC greatly affects the shape of the nano silver, and when the TSC volume is 0.5mL, the sphericity and dispersibility of the nano silver are optimal, and the average particle diameter is about 56.71nm.
In examples 2, 4 and 5, polyvinylpyrrolidone (K30) 0.3-1.0 mL (0.0175 mol/L) was used as a variable, and the PVP as a dispersant had a certain influence on the particle size and dispersion uniformity. Along with the increase of the dispersing agent, the particle size of the nano silver particles has an optimal PVP usage amount, so that the particle size distribution of the nano silver is more balanced. The polydispersity index of the nanosilver solution is the smallest, i.e., the particle size distribution is the narrowest, at a PVP volume of 0.6 mL. In examples 2 and 6, the TEM image of fig. 2 shows that the nano silver changes its shape from spherical to bar-like with the increase of ascorbic acid, taking ascorbic acid 0.2 to 0.5. 0.5mL (0.1 mol/L) as a variable, and the average particle diameter and polydispersity index of the nano silver solution increase.
In examples 2, 7 and 8, 0.2 (0.1 mol/L) ascorbic acid, 0.2mL (0.1 mol/L) sodium borohydride and 0.2mL (0.1M) glucose were used as reducing agents, respectively, and the nanosilver solution prepared from glucose was found to have the smallest polydispersity index, but the average particle size was larger, and the nanosilver prepared from sodium borohydride had the largest average particle size.
According to the invention, the particle size distribution, the average particle size and the polydispersity index of the nano silver solution are closely related to the types and the usage amounts of the protective agent, the dispersing agent and the reducing agent, 50mL of ultrapure water is sequentially added with 50 mu L (0.05 mol/L), 0.5mL (0.075 mol/L) of sodium citrate (TSC) and 0.6mL (0.0175 mol/L) of polyvinylpyrrolidone, and the mixture is rapidly stirred and uniformly dispersed at the rotating speed of 400r/min, 0.2mL (0.1 mol/L) of ascorbic acid is added after 3min, and the mixture is continuously stirred for 30min to obtain the spherical nano silver solution with good dispersibility and narrow particle size distribution.
It will be apparent that the embodiments described above are only some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Claims (2)
1. The preparation method of the mild condition controllable nano silver solution is characterized by comprising the following steps of: the method comprises the steps of taking ultrapure water as a solvent, taking 99.95% silver nitrate as a silver source, taking sodium citrate as a protective agent, taking polyvinylpyrrolidone as a dispersing agent and taking ascorbic acid as a reducing agent, sequentially adding 0.05mol/L silver nitrate 50 mu L, 0.075mol/L sodium citrate 0.3-0.5 mL and 0.0175mol/L polyvinylpyrrolidone 0.6mL into 50mL of ultrapure water at room temperature, stirring for 3min at the rotating speed of 400r/min, adding 0.1mol/L reducing agent 0.2mL, and continuously stirring for reacting for 30min to obtain the nano silver solution with the particle size of 60nm and the shape of a sphere.
2. The method for preparing the mild condition controllable nano-silver solution according to claim 1, wherein the molar ratio of sodium citrate to silver nitrate is 9-15:1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111361819.7A CN114160785B (en) | 2021-11-17 | 2021-11-17 | Preparation method of mild condition controllable nano silver solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111361819.7A CN114160785B (en) | 2021-11-17 | 2021-11-17 | Preparation method of mild condition controllable nano silver solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114160785A CN114160785A (en) | 2022-03-11 |
| CN114160785B true CN114160785B (en) | 2024-01-26 |
Family
ID=80479397
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111361819.7A Active CN114160785B (en) | 2021-11-17 | 2021-11-17 | Preparation method of mild condition controllable nano silver solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114160785B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115846648B (en) * | 2022-12-13 | 2023-10-31 | 武汉船用电力推进装置研究所（中国船舶重工集团公司第七一二研究所） | High-activity spherical silver powder with cracking-shaped rough surface structure and preparation method thereof |
Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009256776A (en) * | 2008-03-27 | 2009-11-05 | Tokyo Printing Ink Mfg Co Ltd | Method for producing silver fine particle |
| CN101731272A (en) * | 2009-12-24 | 2010-06-16 | 中国人民解放军军事医学科学院基础医学研究所 | Method for preparing antibacterial nanometer silver colloid |
| KR20100115201A (en) * | 2009-04-17 | 2010-10-27 | 웅진케미칼 주식회사 | Nano-silver controled particles size and preparing thereof |
| CN101885072A (en) * | 2010-07-01 | 2010-11-17 | 苏州永拓环境科技有限公司 | Preparation method of nano-silver sol |
| CN102407342A (en) * | 2011-10-31 | 2012-04-11 | 山东大学 | Preparation method of nano silver powder with accurately controllable particle size |
| CN102489717A (en) * | 2011-12-22 | 2012-06-13 | 云南云天化股份有限公司 | Preparation method of nanometer silver particles |
| WO2014058904A1 (en) * | 2012-10-11 | 2014-04-17 | Nanocomposix, Inc. | Silver nanoplate compositions and methods |
| CN104400000A (en) * | 2014-11-07 | 2015-03-11 | 中国船舶重工集团公司第七一二研究所 | Method for preparing spherical silver powder |
| KR20150048295A (en) * | 2013-10-25 | 2015-05-07 | 한국과학기술원 | Synthesis method for AuNPCs with tuned size and shape |
| CN104646683A (en) * | 2015-02-28 | 2015-05-27 | 湖南汇通科技有限责任公司 | Spherical silver powder with controllable granularity and preparation method thereof |
| KR20150071423A (en) * | 2013-12-18 | 2015-06-26 | 주식회사 나노신소재 | Method of manufacturing nanowires |
| CN105252019A (en) * | 2015-11-20 | 2016-01-20 | 济南大学 | Preparation method of highly-dispersed spherical nano-silver |
| KR20180108537A (en) * | 2018-09-21 | 2018-10-04 | 경희대학교 산학협력단 | Method for manufacturing silver nanocube-particles and silver nanocube-particles manufactured by the same |
| CN111097922A (en) * | 2020-02-21 | 2020-05-05 | 深圳先进技术研究院 | Nano silver particle and preparation method and application thereof |
| CN111922358A (en) * | 2020-09-24 | 2020-11-13 | 东北大学 | Method for synthesizing nano silver with controllable morphology by reduction at normal temperature |
| CN111992738A (en) * | 2020-09-19 | 2020-11-27 | 西安瑞特三维科技有限公司 | Method for synthesizing nano silver particles with wide range of particle size distribution by one-pot method |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20130192423A1 (en) * | 2012-01-27 | 2013-08-01 | Blue Nano Inc. | Method of producing silver nanowires |
| JP2020183567A (en) * | 2019-05-08 | 2020-11-12 | トヨタ自動車株式会社 | Method for producing silver nanoparticle |
-
2021
- 2021-11-17 CN CN202111361819.7A patent/CN114160785B/en active Active
Patent Citations (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009256776A (en) * | 2008-03-27 | 2009-11-05 | Tokyo Printing Ink Mfg Co Ltd | Method for producing silver fine particle |
| KR20100115201A (en) * | 2009-04-17 | 2010-10-27 | 웅진케미칼 주식회사 | Nano-silver controled particles size and preparing thereof |
| CN101731272A (en) * | 2009-12-24 | 2010-06-16 | 中国人民解放军军事医学科学院基础医学研究所 | Method for preparing antibacterial nanometer silver colloid |
| CN101885072A (en) * | 2010-07-01 | 2010-11-17 | 苏州永拓环境科技有限公司 | Preparation method of nano-silver sol |
| CN102407342A (en) * | 2011-10-31 | 2012-04-11 | 山东大学 | Preparation method of nano silver powder with accurately controllable particle size |
| CN102489717A (en) * | 2011-12-22 | 2012-06-13 | 云南云天化股份有限公司 | Preparation method of nanometer silver particles |
| WO2014058904A1 (en) * | 2012-10-11 | 2014-04-17 | Nanocomposix, Inc. | Silver nanoplate compositions and methods |
| KR20150048295A (en) * | 2013-10-25 | 2015-05-07 | 한국과학기술원 | Synthesis method for AuNPCs with tuned size and shape |
| KR20150071423A (en) * | 2013-12-18 | 2015-06-26 | 주식회사 나노신소재 | Method of manufacturing nanowires |
| CN104400000A (en) * | 2014-11-07 | 2015-03-11 | 中国船舶重工集团公司第七一二研究所 | Method for preparing spherical silver powder |
| CN104646683A (en) * | 2015-02-28 | 2015-05-27 | 湖南汇通科技有限责任公司 | Spherical silver powder with controllable granularity and preparation method thereof |
| CN105252019A (en) * | 2015-11-20 | 2016-01-20 | 济南大学 | Preparation method of highly-dispersed spherical nano-silver |
| KR20180108537A (en) * | 2018-09-21 | 2018-10-04 | 경희대학교 산학협력단 | Method for manufacturing silver nanocube-particles and silver nanocube-particles manufactured by the same |
| CN111097922A (en) * | 2020-02-21 | 2020-05-05 | 深圳先进技术研究院 | Nano silver particle and preparation method and application thereof |
| CN111992738A (en) * | 2020-09-19 | 2020-11-27 | 西安瑞特三维科技有限公司 | Method for synthesizing nano silver particles with wide range of particle size distribution by one-pot method |
| CN111922358A (en) * | 2020-09-24 | 2020-11-13 | 东北大学 | Method for synthesizing nano silver with controllable morphology by reduction at normal temperature |
Non-Patent Citations (4)
| Title |
|---|
| 化学还原法制备纳米银颗粒即纳米银导电浆料的性能;王小叶;《贵金属》;14-19 * |
| 聚乙烯吡咯烷酮与柠檬酸钠的加入量对葡萄糖还原法制备Cu2O颗粒形貌的影响;杨宇婷;《青岛科技大学学报》;121-125 * |
| 银纳米立方体的制备及其影响因素;王悦辉;《材料导报》;144-147 * |
| 高浓度体系下银粉形貌和结构的还原剂与分散剂影响研究;孙宝;《船电技术》;61-64 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114160785A (en) | 2022-03-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109128211B (en) | Method for preparing micro-nano silver particles in aqueous solution system | |
| CN103567431B (en) | A kind of nano-class silver colloidal solution and preparation method thereof | |
| US20120225126A1 (en) | Solid state synthesis method of silver nanoparticles, and silver nanoparticles synthesized thereby | |
| Mohammadi et al. | Green synthesis, characterization and antimicrobial activity of silver nanoparticles (AgNPs) using leaves and stems extract of some plants | |
| US20210261418A1 (en) | Method for synthesizing high-purity carbon nanocoils based on composite catalyst formed by multiple small-sized catalyst particles | |
| CN108620601B (en) | Method for preparing flaky Cu nanocrystalline at room temperature | |
| CN114160785B (en) | Preparation method of mild condition controllable nano silver solution | |
| Jawaad et al. | Synthesis of silver nanoparticles | |
| CN103071808A (en) | Environmentally-friendly synthetic method for metal nanoparticle | |
| CN113275011B (en) | Preparation method of cuprous oxide photocatalyst with flower-ball-shaped multi-stage structure | |
| Pedroza-Toscano et al. | Silver nanoparticles obtained by semicontinuous chemical reduction using carboxymethyl cellulose as a stabilizing agent and its antibacterial capacity | |
| CN111992734B (en) | Preparation method of nano-silver with controllable particle size | |
| CN109676149B (en) | Green synthetic wheat gliadin/nano-silver particle with core-shell structure and preparation method and application thereof | |
| CN111872410A (en) | Preparation method of nano platinum | |
| CN113044874B (en) | Method for preparing small-size CuBr nanoparticles by liquid phase method | |
| Gu et al. | Effect of aqueous ammonia addition on the morphology and size of silver particles reduced by ascorbic acid | |
| CN111992738B (en) | Method for synthesizing nano silver particles with wide range of particle size distribution by one-pot method | |
| CN113814408A (en) | Preparation of CuPd alloy nanocrystalline and component regulation and control method thereof | |
| WO2023227145A1 (en) | Preparation method for platinum nanoparticles, platinum nanoparticles prepared therefrom, and application of platinum nanoparticles | |
| CN111347060A (en) | Preparation method of nano-silver colloid with controllable particle size | |
| CN108213459B (en) | Preparation method of glucan/nano gold-silver alloy compound | |
| Guo et al. | Preparation of gold nanoparticles on nanocellulose and their catalytic activity for reduction of NO2 | |
| Zhang et al. | " Green" synthesis of size controllable Prussian blue nanoparticles stabilized by soluble starch | |
| Cheng et al. | Facile synthesis of CQDs/Ag NPs composites with photoluminescence and their potential application in antibacterial materials | |
| CN111096334A (en) | Preparation method of GSH (glutathione) modified silver sulfide nano-cluster antibacterial material and silver sulfide nano-cluster antibacterial material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |