CN110976910A - Size-adjustable nano silver and synthetic method and application thereof - Google Patents
Size-adjustable nano silver and synthetic 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 76
- 238000010189 synthetic method Methods 0.000 title claims abstract description 8
- 239000004332 silver Substances 0.000 claims abstract description 30
- 229910052709 silver Inorganic materials 0.000 claims abstract description 30
- -1 silver ions Chemical class 0.000 claims abstract description 28
- 238000000034 method Methods 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 26
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001308 synthesis method Methods 0.000 claims abstract description 21
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 11
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 11
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000005642 Oleic acid Substances 0.000 claims abstract description 11
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 11
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 11
- 229930006000 Sucrose Natural products 0.000 claims abstract description 11
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 11
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 11
- 239000005720 sucrose Substances 0.000 claims abstract description 11
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000003651 drinking water Substances 0.000 claims abstract description 4
- 235000020188 drinking water Nutrition 0.000 claims abstract description 4
- 239000002904 solvent Substances 0.000 claims abstract description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 24
- 239000007787 solid Substances 0.000 claims description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 238000000746 purification Methods 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001514 detection method Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 238000000926 separation method Methods 0.000 claims description 3
- 230000002194 synthesizing effect Effects 0.000 claims description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 7
- 230000001105 regulatory effect Effects 0.000 abstract description 4
- 239000003381 stabilizer Substances 0.000 abstract description 4
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 238000004729 solvothermal method Methods 0.000 abstract 1
- 230000000087 stabilizing effect Effects 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 35
- 238000010521 absorption reaction Methods 0.000 description 7
- 230000007423 decrease Effects 0.000 description 7
- 238000004108 freeze drying Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 238000010992 reflux Methods 0.000 description 6
- 238000003917 TEM image Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003446 ligand Substances 0.000 description 3
- 230000035040 seed growth Effects 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 2
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000003223 protective agent Substances 0.000 description 2
- 239000012279 sodium borohydride Substances 0.000 description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 238000001479 atomic absorption spectroscopy Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000001095 inductively coupled plasma mass spectrometry Methods 0.000 description 1
- 238000002354 inductively-coupled plasma atomic emission spectroscopy Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003445 sucroses Chemical class 0.000 description 1
- 238000004846 x-ray emission Methods 0.000 description 1
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- B22—CASTING; POWDER METALLURGY
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- 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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- 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
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/33—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using ultraviolet light
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Abstract
The invention belongs to the technical field of nanometer, and particularly relates to nano-silver with adjustable size, a synthetic method and application thereof. Carbon dots are simultaneously used as a reducing agent and a stabilizing agent to prepare the nano silver with adjustable size at room temperature. The surface of the carbon dot contains a large amount of hydroxyl and carboxyl, has the capability of reducing silver ions, and can be matched with silver to play a role in stabilizing nano silver. The synthesis method comprises two steps, wherein in the first step, a solvothermal method is utilized, sucrose is used as a carbon source, oleic acid is used as a hot solvent, carbon points with hydroxyl and carboxyl on the surface are synthesized, and in the second step, silver ion solutions with different amounts are added into an alkaline carbon point solution, so that the nano silver with adjustable size can be obtained. The nano silver synthesized by the method has good dispersibility and size unicity, and the size of the nano silver is finely regulated and controlled between 3.5 nm and 35.2nm by simply changing the pH value of the system and the concentration of silver ions. The method for preparing the nano silver can be used for detecting the content of silver ions in a drinking water system.
Description
Technical Field
The invention belongs to the technical field of nanometer, and particularly relates to nano-silver with adjustable size, a synthetic method and application thereof.
Background
Silver and its composite materials have very important roles in many industrial processes and industrial products, and they are widely used as catalysts, electrodes, antibacterial agents, etc. The nano silver is mainly prepared by a micro-emulsion method, a sonochemical reduction method, a photochemical method and the like. However, these synthetic methods are often time consuming and require expensive instrumentation. In the synthesis process of nano silver, sodium borohydride is generally selected as a reducing agent, however, sodium borohydride has very strong reducing capability, so that the reaction process is difficult to control, and in order to overcome the problems, a novel reducing agent and a novel stabilizing agent need to be developed for the synthesis of nano silver. Silver ions can be slowly released by the silver-containing material in the using process, and the negative influence is caused on human health and ecological environment. Therefore, for drinking water, food and ecological safety, it is necessary to detect the content in the environment, particularly in the water system, using a simple, efficient and rapid method. In general, researchers use atomic absorption spectroscopy, inductively coupled plasma atomic emission spectroscopy, inductively coupled plasma mass spectrometry, X-ray fluorescence spectroscopy, and other methods to detect the content of silver ions.
The traditional method for regulating the size of the nano-silver is mainly a seed growth method, the seed growth method is time-consuming to operate, and the size regulation is not fine enough. Patent CN201811370210.4 discloses a method for preparing nano silver particles by using modified sucrose as a reducing agent and a protective agent and reducing silver nitrate, and the patent adopts a modification method to prepare nano silver, and the size of the nano silver cannot be adjusted and cannot be used for detecting silver ions.
Other methods for detecting silver ions often require complex procedures and expensive instrumentation. Therefore, it is necessary to develop a method for detecting silver ions simply and rapidly at low cost.
Disclosure of Invention
In order to solve the technical problems, the invention provides nano silver with adjustable size and a synthesis method and application thereof.
The technical scheme of the invention is realized as follows:
a synthetic method of nano silver with adjustable size comprises the following steps:
(1) selecting sucrose as a carbon source and oleic acid as a hot solvent, uniformly mixing, and then carrying out heating reaction, separation and purification to obtain carbon dots;
(2) preparing a carbon dot solution from the carbon dots obtained in the step (1), adding sodium hydroxide to adjust the pH value, and then adding a silver nitrate solution to react for a period of time under the condition of stirring at room temperature to obtain the nano silver with adjustable size.
In the step (1), 2-5mL of oleic acid is added per g of sucrose.
The heating reaction in the step (1) is carried out under the condition that the temperature of the reaction system is heated to 205 ℃ and 215 ℃ at the speed of 8 ℃/min, and the reaction is carried out for 1-5 min.
And (2) cooling the system subjected to the heating reaction to room temperature, removing the upper-layer liquid, adding water to dissolve the solid formed by cooling, extracting for 3 times by using n-hexane, collecting a water-phase product, dialyzing, and freeze-drying to obtain the carbon dot solid.
The concentration of the carbon dot solution in the step (2) is 125 mu g/mL, and the reaction concentration of the silver ions is 100 mu M-8 mM.
The mass ratio of the carbon dots to the silver ions is (0.145-11.57): 1.
in the step (2), the pH value is 11-13, and the reaction time is 3-120 min.
The nano silver with adjustable size prepared by the synthesis method.
The purification method of the nano silver prepared by the synthesis method comprises the following steps: and centrifuging and ultrafiltering the nano silver solution obtained by the reaction, and collecting the interception product, namely the nano silver.
The application of the nano silver with adjustable size in the detection of the content of silver ions in a drinking water system.
The invention has the following beneficial effects:
1. compared with the traditional method for regulating the size of the nano-silver by a seed growth method, the method takes silver nitrate as a silver source, utilizes carbon dots as a reducing agent and a stabilizing agent at the same time, and reacts for a period of time at room temperature in an alkaline solution to obtain the nano-silver with the adjustable size. The method is simple to operate and rapid to prepare, and the nano silver can be obtained in 3 min. According to the method, the carbon dots are simultaneously used as the reducing agent and the protective agent to prepare the nano silver, and the synthesis of the nano silver size is finely regulated and controlled within a small size range.
2. The synthetic method has the advantages that reactants are very simple, only carbon dots, silver nitrate and sodium hydroxide are needed, the reaction temperature is very mild and room temperature is needed, the cost for synthesizing the nano-silver can be greatly reduced, the reaction time is very short, and the nano-silver can be prepared in 3 min.
3. The method successfully adopts the carbon dots as a reducing agent and a stabilizing agent, reduces silver ions by utilizing hydroxyl and carboxyl on the surfaces of the carbon dots, and simultaneously stabilizes the generated nano silver to prepare the nano silver with adjustable size. The size of the synthesized nano silver can be finely adjusted between 3.5-35.2 nm.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a transmission electron micrograph of the nanosilver of example 1.
FIG. 2 is a transmission electron micrograph of the nano-silver of example 2.
FIG. 3 is a transmission electron micrograph of the nano-silver of example 3.
FIG. 4 is a graph showing the UV-VIS absorption spectrum of nano-silver of example 4.
FIG. 5 is a graph showing the UV-VIS absorption spectrum of nano-silver of example 5.
FIG. 6 is a graph showing an ultraviolet-visible absorption spectrum of nano-silver of example 6.
Fig. 7 is a detection diagram of a method for synthesizing nano silver for detecting silver ions in an aqueous system according to an embodiment.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
Example 1
The synthesis method of the size-adjustable nano silver comprises the following steps:
stirring and mixing 5 g of sucrose and 10 mL of oleic acid uniformly, heating the system to 210 ℃ at the speed of 8 ℃/min, condensing and refluxing for 5min, removing upper-layer liquid after the temperature of the system is cooled to room temperature, adding water to dissolve the cooled solid, extracting for 3 times by using normal hexane, collecting a water phase product, dialyzing, and freeze-drying to obtain the carbon dot solid.
Weighing solid carbon dots to prepare a 125 mu g/mL carbon dot solution, adding a sodium hydroxide solution to enable the pH value of the solution to be 13, adding a silver nitrate solution under the stirring condition to enable the silver ion concentration to be 100 mu mol/L, reacting for 3 min to obtain the nano silver with the size of 3.5 nm, wherein a transmission electron microscope picture is shown as figure 1.
Example 2
The synthesis method of the size-adjustable nano silver comprises the following steps:
stirring and mixing 5 g of sucrose and 10 mL of oleic acid uniformly, heating the system to 210 ℃ at the speed of 8 ℃/min, condensing and refluxing for 5min, removing upper-layer liquid after the temperature of the system is cooled to room temperature, adding water to dissolve the cooled solid, extracting for 3 times by using normal hexane, collecting a water phase product, dialyzing, and freeze-drying to obtain the carbon dot solid.
Weighing solid carbon dots to prepare a 125 mu g/mL carbon dot solution, adding a sodium hydroxide solution to enable the pH value of the solution to be 12, adding a silver nitrate solution under the stirring condition to enable the silver ion concentration to be 100 mu mol/L, reacting for 3 min to obtain the nano silver with the size of 6.5 nm, wherein a transmission electron microscope picture is shown as figure 2.
Example 3
The synthesis method of the size-adjustable nano silver comprises the following steps:
stirring and mixing 5 g of sucrose and 10 mL of oleic acid uniformly, heating the system to 210 ℃ at the speed of 8 ℃/min, condensing and refluxing for 5min, removing upper-layer liquid after the temperature of the system is cooled to room temperature, adding water to dissolve the cooled solid, extracting for 3 times by using normal hexane, collecting a water phase product, dialyzing, and freeze-drying to obtain the carbon dot solid.
Weighing solid carbon dots to prepare a 125 mu g/mL carbon dot solution, adding a sodium hydroxide solution to enable the pH value of the solution to be 11, adding a silver nitrate solution under the stirring condition to enable the silver ion concentration to be 100 mu mol/L, reacting for 8 min to obtain the nano silver with the size of 7.4nm, wherein a transmission electron microscope picture is shown as a picture in figure 3. As the pH of the reaction is lowered, the time required for the reaction is longer because the reducing power of the carbon site is lowered. Meanwhile, the size of the produced nano silver decreases with the increase of pH, which is caused by rapid nucleation and growth of nano silver under the high pH condition.
Example 4
The synthesis method of the size-adjustable nano silver comprises the following steps:
stirring and mixing 5 g of sucrose and 10 mL of oleic acid uniformly, heating the system to 210 ℃ at the speed of 8 ℃/min, condensing and refluxing for 5min, removing upper-layer liquid after the temperature of the system is cooled to room temperature, adding water to dissolve the cooled solid, extracting for 3 times by using normal hexane, collecting a water phase product, dialyzing, and freeze-drying to obtain the carbon dot solid.
Weighing solid carbon dots to prepare a 125 mu g/mL carbon dot solution, adding a sodium hydroxide solution to enable the pH value of the solution to be 11, adding a silver nitrate solution under the stirring condition to enable the silver ion concentration to be 100 mu M-8 mM, and reacting for 120 min to obtain the nano silver with the size of 7.4-16.8 nm, wherein an ultraviolet-visible absorption spectrogram is shown in a figure 4. As the concentration of silver ions increases, the size of nano silver gradually increases, and the ultraviolet-visible absorption peak position gradually red shifts, because the mass ratio of carbon dots to silver ions decreases, resulting in a decrease in the relative content of the ligand.
Example 5
The synthesis method of the size-adjustable nano silver comprises the following steps:
stirring and mixing 5 g of sucrose and 10 mL of oleic acid uniformly, heating the system to 210 ℃ at the speed of 8 ℃/min, condensing and refluxing for 5min, removing upper-layer liquid after the temperature of the system is cooled to room temperature, adding water to dissolve the cooled solid, extracting for 3 times by using normal hexane, collecting a water phase product, dialyzing, and freeze-drying to obtain the carbon dot solid.
Weighing solid carbon dots to prepare a 125 mu g/mL carbon dot solution, adding a sodium hydroxide solution to enable the pH value of the solution to be 12, adding a silver nitrate solution under the stirring condition to enable the silver ion concentration to be 100 mu M-8 mM, reacting for 120 min to obtain the nano silver with the size of 6.5-35.2nm, wherein an ultraviolet-visible absorption spectrogram is shown in figure 5. As the concentration of silver ions increases, the size of nano silver gradually increases, and the ultraviolet-visible absorption peak position gradually red shifts, because the mass ratio of carbon dots to silver ions decreases, resulting in a decrease in the relative content of the ligand.
Example 6
The synthesis method of the size-adjustable nano silver comprises the following steps:
stirring and mixing 5 g of sucrose and 10 mL of oleic acid uniformly, heating the system to 210 ℃ at the speed of 8 ℃/min, condensing and refluxing for 5min, removing upper-layer liquid after the temperature of the system is cooled to room temperature, adding water to dissolve the cooled solid, extracting for 3 times by using normal hexane, collecting a water phase product, dialyzing, and freeze-drying to obtain the carbon dot solid.
Weighing solid carbon dots to prepare a 125 mu g/mL carbon dot solution, adding a sodium hydroxide solution to enable the pH value of the solution to be 13, adding a silver nitrate solution under the stirring condition to enable the silver ion concentration to be 100 mu M-4mM, reacting for 120 min to obtain the nano silver with the size of 3.5-21.2 nm, wherein an ultraviolet-visible absorption spectrogram is shown in figure 6. As the concentration of silver ions increases, the size of nano silver gradually increases, and the ultraviolet-visible absorption peak position gradually red shifts, because the mass ratio of carbon dots to silver ions decreases, resulting in a decrease in the relative content of the ligand.
Examples of the effects of the invention
The method of nano silver prepared in example 1 is used for detecting silver ions in a water system.
Weighing solid carbon dots to prepare a 125 mu g/mL carbon dot solution, adding a sodium hydroxide solution to enable the pH value of the solution to be 13, adding a silver nitrate solution under the stirring condition to enable the final concentration of silver ions to be 0-100 mu M, uniformly stirring the mixed solution for 3 min, measuring the ultraviolet-visible absorption spectrum of the mixed solution by using a MAPADA double-beam spectrophotometer, reading the absorbance value of the nano-silver at an absorption peak of 409nm, and establishing a standard curve of the absorbance value to the concentration of the silver ions, wherein as shown in FIG. 7, whether the sample to be detected contains the silver ions can be determined by using the nano-silver characteristic diagram of FIG. 7.
The east lake water is centrifuged at 10000 rpm, then is filtered by using a 0.22 mu m filter head, a water sample is digested by nitric acid, and the concentration of silver ions in the solution is detected by using the method and a standard-adding recovery method.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (9)
1. A synthetic method of nano silver with adjustable size is characterized by comprising the following steps:
(1) selecting sucrose as a carbon source and oleic acid as a hot solvent, uniformly mixing, and then carrying out heating reaction, separation and purification to obtain carbon dots;
(2) preparing a carbon dot solution from the carbon dots obtained in the step (1), adding sodium hydroxide to adjust the pH value, and then adding a silver nitrate solution to react for a period of time under the condition of stirring at room temperature to obtain the nano silver with adjustable size.
2. The synthesis method of the nano silver with adjustable size as claimed in claim 1, wherein the synthesis method comprises the following steps: in the step (1), 2-5mL of oleic acid is added per g of sucrose.
3. The synthesis method of the nano silver with adjustable size as claimed in claim 2, wherein the synthesis method comprises the following steps: the heating reaction in the step (1) is carried out under the condition that the temperature of the reaction system is heated to 205 ℃ and 215 ℃ at the speed of 8 ℃/min, and the reaction is carried out for 1-5 min.
4. The method for synthesizing size-adjustable nano silver according to claim 1, wherein the separation and purification in step (1) comprises cooling the system after the heating reaction to room temperature, removing the upper liquid layer, dissolving the cooled solid in water, extracting with n-hexane for 3 times, collecting the water phase product, dialyzing, and lyophilizing to obtain the carbon dot solid.
5. The synthesis method of the nano silver with adjustable size as claimed in claim 1, wherein the synthesis method comprises the following steps: the concentration of the carbon dot solution in the step (2) is 125 mu g/mL, and the reaction concentration of the silver ions is 100 mu M-8 mM.
6. The synthesis method of the nano silver with adjustable size as claimed in claim 5, wherein the synthesis method comprises the following steps: the mass ratio of the carbon dots to the silver ions is (0.145-11.57): 1.
7. the synthesis method of the nano silver with adjustable size as claimed in claim 1, wherein the synthesis method comprises the following steps: in the step (2), the pH value is 11-13, and the reaction time is 3-120 min.
8. The size-adjustable nano silver prepared by the synthesis method of any one of claims 1 to 7.
9. The use of the nano silver with adjustable size as claimed in claim 8 in the detection of silver ion content in drinking water system.
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Citations (6)
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| US20100154591A1 (en) * | 2008-12-23 | 2010-06-24 | Islam M Rafiq | Household microwave-mediated carbohydrate-based production of silver nanomaterials |
| RS20110073A2 (en) * | 2011-02-09 | 2012-08-31 | Institut Tehniäśkih Nauka Srpske Akademije Nauka I Umetnosti | Process of obtaining multifunctional micro and nanocomposite spheres with silver nanoparticles coated with biodegradable polymers |
| KR20140027786A (en) * | 2012-08-27 | 2014-03-07 | 강원대학교산학협력단 | Preparation method of silver nano-structure for surface enhanced raman scattering substrate and silver nano-structure thereby |
| CN106053408A (en) * | 2016-05-17 | 2016-10-26 | 无锡市疾病预防控制中心 | Carbon dot fluorescent probe based high sensitive and high selective method for detecting trace silver nano particles in water and/or environment |
| CN106645035A (en) * | 2016-12-16 | 2017-05-10 | 盐城工学院 | Method for detecting content of heavy metal silver ions based on carbon-spot light scattering sensing |
| CN107216873A (en) * | 2017-05-19 | 2017-09-29 | 辽宁大学 | A kind of preparation method and applications for being used to detect the carbon point of silver ion and dimercaptosuccinic acid |
-
2020
- 2020-01-14 CN CN202010035570.XA patent/CN110976910A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100154591A1 (en) * | 2008-12-23 | 2010-06-24 | Islam M Rafiq | Household microwave-mediated carbohydrate-based production of silver nanomaterials |
| RS20110073A2 (en) * | 2011-02-09 | 2012-08-31 | Institut Tehniäśkih Nauka Srpske Akademije Nauka I Umetnosti | Process of obtaining multifunctional micro and nanocomposite spheres with silver nanoparticles coated with biodegradable polymers |
| KR20140027786A (en) * | 2012-08-27 | 2014-03-07 | 강원대학교산학협력단 | Preparation method of silver nano-structure for surface enhanced raman scattering substrate and silver nano-structure thereby |
| CN106053408A (en) * | 2016-05-17 | 2016-10-26 | 无锡市疾病预防控制中心 | Carbon dot fluorescent probe based high sensitive and high selective method for detecting trace silver nano particles in water and/or environment |
| CN106645035A (en) * | 2016-12-16 | 2017-05-10 | 盐城工学院 | Method for detecting content of heavy metal silver ions based on carbon-spot light scattering sensing |
| CN107216873A (en) * | 2017-05-19 | 2017-09-29 | 辽宁大学 | A kind of preparation method and applications for being used to detect the carbon point of silver ion and dimercaptosuccinic acid |
Non-Patent Citations (3)
| Title |
|---|
| JIAN-CHENG JIN等: "A novel method for the detection of silver ions with carbon dots Excellent selectivity, fast response, low detection limit and good applicability", 《SENSORS AND ACTUATORS B: CHEMICAL》 * |
| JIAN-CHENG JIN等: "One-step synthesis of silver nanoparticles using carbon dots as reducing and stabilizing agents and their antibacterial mechanisms", 《CARBON》 * |
| 边照阳等: "正己烷", 《QUECHERS技术及应用》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113245556A (en) * | 2021-05-10 | 2021-08-13 | 福州大学 | Dimension-controllable aggregation-state nano silver and preparation method thereof |
| CN113245556B (en) * | 2021-05-10 | 2022-06-21 | 福州大学 | Dimension-controllable aggregation-state nano silver and preparation method thereof |
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