CN115090893B - Method for preparing nano silver with controllable size - Google Patents
Method for preparing nano silver with controllable size Download PDFInfo
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- CN115090893B CN115090893B CN202210634938.3A CN202210634938A CN115090893B CN 115090893 B CN115090893 B CN 115090893B CN 202210634938 A CN202210634938 A CN 202210634938A CN 115090893 B CN115090893 B CN 115090893B
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- silver
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- soluble starch
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 238000000034 method Methods 0.000 title claims abstract description 16
- 229920002472 Starch Polymers 0.000 claims abstract description 39
- 239000008107 starch Substances 0.000 claims abstract description 39
- 235000019698 starch Nutrition 0.000 claims abstract description 39
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 102000004139 alpha-Amylases Human genes 0.000 claims abstract description 20
- 108090000637 alpha-Amylases Proteins 0.000 claims abstract description 20
- 229940024171 alpha-amylase Drugs 0.000 claims abstract description 20
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- 239000002245 particle Substances 0.000 claims description 20
- 230000001276 controlling effect Effects 0.000 claims description 18
- 229910052709 silver Inorganic materials 0.000 claims description 10
- 239000004332 silver Substances 0.000 claims description 10
- -1 silver ions Chemical class 0.000 claims description 10
- 238000009835 boiling Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 238000004090 dissolution Methods 0.000 claims 1
- 238000002360 preparation method Methods 0.000 abstract description 7
- 239000002270 dispersing agent Substances 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- 239000007864 aqueous solution Substances 0.000 description 11
- 239000003638 chemical reducing agent Substances 0.000 description 11
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 9
- 239000000284 extract Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 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 3
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 2
- 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 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
- 239000013078 crystal Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 229920005862 polyol Polymers 0.000 description 2
- 150000003077 polyols Chemical class 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000002147 killing effect Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000004917 polyol method Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 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 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 238000009827 uniform distribution Methods 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
- B22F1/0545—Dispersions or suspensions of nanosized particles
-
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Physics & Mathematics (AREA)
- Composite Materials (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a method for preparing nano silver with controllable size, which uses silver nitrate, soluble starch and alpha amylase as raw materials to prepare nano silver under the irradiation of light with precisely controlled frequency. The preparation method of the invention realizes the accurate preparation of the nano silver size of 3-100 nm by controlling the frequency of light. The preparation method of the nano silver does not use PVP dispersing agent, is environment-friendly, and the prepared nano silver has accurate and controllable size and good singleness.
Description
Technical Field
The invention belongs to the technical field of new material preparation, and particularly relates to a preparation method of nano silver.
Background
Nano silver refers to a silver simple substance with at least one dimension between 1 and 100 nanometers, and can be zero-dimensional particles, one dimension such as nano silver wires, two-dimensional nano silver films and the like. The nano silver material is widely used in the fields of biological medicine, semiconductors and the like. The application in the aspect of biological medicine is mainly based on the spectrum killing effect of nano silver on various bacteria, fungi, viruses and other microorganisms. The nano silver is one of the nano materials with the largest dosage as the antibacterial material.
The preparation method of nano silver generally utilizes various substances with reducibility to reduce soluble silver salt mainly silver nitrate, and the reducing agent can be divided into chemical reducing agents and biological extract reducing agents, wherein the chemical reducing agents specifically utilize various substances with reducibility such as sodium borohydride, hydrazine hydrate, polyalcohol, ascorbic acid, glucose, sodium citrate and the like; in order to control the particle size of nano silver, a dispersant is generally added by using a reducing agent, and in this case, as an example, a polyol method is used, PVP is generally added as a dispersant for reducing nano silver by using a polyol, and the dosage of the dispersant needs the dosage of excessive reducing agent polyol, so that toxic and harmful PVP and the like are introduced, and parameters which can be controlled by a chemical reduction method for obtaining high-quality nano silver are generally: the concentration, the dosage, the use proportion and the like of the reducing agent and the silver salt are very difficult to obtain the nano silver with controllable particle size and uniform distribution. Biological extracts are reported in literature, and extracts such as rhizome and leaf of various plants are used as reducing agents to reduce silver salt to prepare nano silver.
Compared with the method that no artificially synthesized toxic or harmful chemical substances are introduced in the method for reducing nano silver by taking the rhizome and leaf extract of the plant as the reducing agent, the biocompatibility of the nano silver can be improved. However, the biological extract used as a reducing agent for reducing the nano silver also has the problems of complex process, low efficiency, too wide particle size distribution of the nano silver reduced by complex components, poor quality and the like.
Disclosure of Invention
The invention aims to provide a method for preparing nano silver with controllable particle size, which aims to solve the problems of poor monodispersity and uncontrollable particle size of the nano silver prepared by the prior art in the background technology. In order to achieve the above purpose, the invention adopts the following technical scheme: the method for preparing the nano silver with controllable particle size comprises the following steps:
Dissolving soluble starch in water, heating, boiling and dissolving to prepare aqueous solution with starch concentration of 60-10000 ppm, cooling to room temperature of 25 ℃, adding silver nitrate to dissolve, controlling silver ion concentration to be 30-5000 ppm, controlling the mass of the soluble starch in the solution to be twice that of silver ions, adding alpha amylase to the solution, stirring and dispersing, keeping the concentration of the alpha amylase to be 0.1% of that of the soluble starch, placing the solution under an adjustable light source with light intensity of 1-10 Wanlex and light wavelength of 200-800 nm for 1-5 hours to obtain nano silver with particle size of 3-80 nm, wherein the formation of nano silver crystal nuclei is promoted by hydrolyzing starch by the alpha amylase to slowly control glucose, and the growth of the nano silver crystal nuclei can be precisely controlled by regulating light intensity and light frequency, thereby controlling the particle size of the nano silver.
The method has the beneficial effects that the method does not use dispersing agents such as PVP and the like, the preparation process is environment-friendly, and the particle size of the nano silver can be accurately controlled.
Drawings
FIG. 1 is a transmission electron microscope image of nano silver obtained in example 4 of the present invention;
FIG. 2 is an EDS spectrum of the nano silver prepared in example 4 of the present invention;
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. 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, remain within the scope of the inventive arrangements.
Example 1:
Dissolving soluble starch in water, heating, boiling and dissolving to prepare aqueous solution with starch concentration of 60ppm, cooling to room temperature of 25 ℃, adding silver nitrate to dissolve, controlling silver ion concentration to be 30ppm, controlling the mass of the soluble starch in the solution to be twice that of silver ions, adding alpha amylase into the solution, stirring and dispersing, keeping the concentration of the alpha amylase to be 0.1% of that of the soluble starch, placing the solution under an adjustable light source with light intensity of 1 Wallows and light wavelength of 800 nanometers for 3 hours to obtain nano silver with particle size of 5 nanometers.
Example 2:
Dissolving soluble starch in water, heating, boiling and dissolving to prepare an aqueous solution with the starch concentration of 200ppm, cooling to the room temperature of 25 ℃, adding silver nitrate into the aqueous solution to dissolve, controlling the silver ion concentration to be 100ppm, controlling the mass of the soluble starch in the solution to be twice that of silver ions, adding alpha amylase into the solution, stirring and dispersing, keeping the alpha amylase concentration to be 0.1% of that of the soluble starch, placing the solution under an adjustable light source with the light intensity of 2 Wallows and the light wavelength of 600 nanometers for 3 hours to obtain the nano silver with the particle size of 60 nanometers.
Example 3:
Dissolving soluble starch in water, heating, boiling and dissolving to prepare aqueous solution with starch concentration of 400ppm, cooling to room temperature of 25 ℃, adding silver nitrate to dissolve, controlling silver ion concentration to be 200ppm, controlling the mass of the soluble starch in the solution to be twice that of silver ions, adding alpha amylase into the solution, stirring and dispersing, keeping the concentration of the alpha amylase to be 0.1% of that of the soluble starch, placing the solution under an adjustable light source with light intensity of 5 Wallows and light wavelength of 500 nm for 3 hours to obtain nano silver with particle size of 40 nm.
Example 4:
Dissolving soluble starch in water, heating, boiling and dissolving to prepare an aqueous solution with the starch concentration of 1000ppm, cooling to the room temperature of 25 ℃, adding silver nitrate into the aqueous solution to dissolve, controlling the silver ion concentration to be 500ppm, controlling the mass of the soluble starch in the solution to be twice that of silver ions, adding alpha amylase into the solution, stirring and dispersing, keeping the alpha amylase concentration to be 0.1% of that of the soluble starch, placing the solution under an adjustable light source with the light intensity of 5 Wallows and the light wavelength of 400 nanometers for 3 hours to obtain the nano silver with the particle size of 30 nanometers.
Example 5:
Dissolving soluble starch in water, heating, boiling and dissolving to prepare aqueous solution with the starch concentration of 2000ppm, cooling to the room temperature of 25 ℃, adding silver nitrate to dissolve, controlling the silver ion concentration to be 1000ppm, controlling the mass of the soluble starch in the solution to be twice that of silver ions, adding alpha amylase into the solution, stirring and dispersing, keeping the alpha amylase concentration to be 0.1% of that of the soluble starch, placing the solution under an adjustable light source with the light intensity of 6 Wallows and the light wavelength of 350 nanometers for 3 hours to obtain nano silver with the particle size of 20 nanometers.
Example 6:
Dissolving soluble starch in water, heating, boiling and dissolving to prepare aqueous solution with the starch concentration of 6000ppm, cooling to the room temperature of 25 ℃, adding silver nitrate into the aqueous solution to dissolve, controlling the silver ion concentration to 3000ppm, controlling the mass of the soluble starch in the solution to be twice that of silver ions, adding alpha amylase into the solution, stirring and dispersing, keeping the alpha amylase concentration to be 0.1% of that of the soluble starch, placing the solution under an adjustable light source with the light intensity of 7 Wallows and the light wavelength of 300 nanometers for 3 hours to obtain the nano silver with the particle size of 10 nanometers.
Example 7:
Dissolving soluble starch in water, heating, boiling and dissolving to prepare aqueous solution with starch concentration of 10000ppm, cooling to room temperature of 25 ℃, adding silver nitrate to dissolve, controlling silver ion concentration to 5000ppm, controlling the mass of the soluble starch in the solution to be twice that of silver ion, adding alpha amylase into the solution, stirring and dispersing, keeping the concentration of the alpha amylase to be 0.1% of that of the soluble starch, placing the solution under an adjustable light source with light intensity of 10 Wallows and light wavelength of 200 nanometers for 3 hours to obtain nano silver with particle size of 3 nanometers.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. A method for preparing nano silver with controllable size, which is characterized by comprising the following steps:
Dissolving soluble starch in water, heating, boiling and dissolving to prepare starch solution, cooling to room temperature of 25 ℃, adding silver nitrate to dissolve, adding alpha amylase to the solution, stirring and dispersing, and placing the solution under a light intensity and wavelength adjustable light source for 3 hours to obtain nano silver with the particle size of 3-80 nanometers, wherein the particle size of the nano silver can be regulated and controlled by controlling the light intensity and wavelength, the light intensity is 1-10 kaleidos, and the wavelength is 200-800 nanometers.
2. A method of preparing nano-silver of controllable size according to claim 1, comprising: the concentration of the prepared starch solution is 60-10000 ppm.
3. A method of preparing nano-silver of controllable size according to claim 1, comprising: after adding silver nitrate for dissolution, the concentration of silver ions is 30-5000 ppm, and the concentration of silver ions is controlled to be half of that of soluble starch.
4. A method of preparing nano-silver of controllable size according to claim 1, comprising: the mass of the added alpha amylase is 0.1% of that of the soluble starch.
5. A method of preparing nano-silver of controllable size according to claim 1, comprising: the smaller the intensity of light, the longer the wavelength, and the larger the particle size of the nano silver.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202210634938.3A CN115090893B (en) | 2022-06-06 | 2022-06-06 | Method for preparing nano silver with controllable size |
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| CN202210634938.3A CN115090893B (en) | 2022-06-06 | 2022-06-06 | Method for preparing nano silver with controllable size |
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| CN115090893A CN115090893A (en) | 2022-09-23 |
| CN115090893B true CN115090893B (en) | 2024-06-25 |
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| CN110640161A (en) * | 2019-10-08 | 2020-01-03 | 厦门医学院 | Method for preparing high-stability nano-silver sol from konjac glucomannan in green manner |
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| JP5139860B2 (en) * | 2008-03-31 | 2013-02-06 | 三菱製紙株式会社 | Method for producing silver ultrafine particles |
| CN104551010B (en) * | 2015-01-19 | 2016-10-26 | 青岛农业大学 | A kind of method preparing water-soluble nano silver for template with short amylose |
| CN105522165B (en) * | 2015-12-17 | 2017-05-24 | 华星美科新材料（江苏）有限公司 | Preparation method for nano-silver particles |
| CN105914242A (en) * | 2016-06-26 | 2016-08-31 | 吴迪 | Method of preparing ultrafine silver powder used by solar cell positive electrode material |
| CN107498067B (en) * | 2017-09-21 | 2019-10-18 | 厦门医学院 | The method that Bao internal organ degradation product green quickly prepares nano silver colloidal sol |
| CN111097921B (en) * | 2020-01-13 | 2021-05-14 | 山西大学 | Anti-colon cancer silver nanoparticles and preparation method thereof |
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| CN110640161A (en) * | 2019-10-08 | 2020-01-03 | 厦门医学院 | Method for preparing high-stability nano-silver sol from konjac glucomannan in green manner |
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