CN111252803A - Square AgCl nanoparticles and preparation method and application thereof - Google Patents
Square AgCl nanoparticles and preparation method and application thereof Download PDFInfo
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- 239000002105 nanoparticle Substances 0.000 title claims abstract description 42
- 229910021607 Silver chloride Inorganic materials 0.000 title claims abstract description 41
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000002086 nanomaterial Substances 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 34
- KYQCOXFCLRTKLS-UHFFFAOYSA-N Pyrazine Chemical compound C1=CN=CC=N1 KYQCOXFCLRTKLS-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 17
- PCNDJXKNXGMECE-UHFFFAOYSA-N Phenazine Natural products C1=CC=CC2=NC3=CC=CC=C3N=C21 PCNDJXKNXGMECE-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 14
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical group Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 238000013329 compounding Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 230000001376 precipitating effect Effects 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000004108 freeze drying Methods 0.000 claims description 3
- 230000002401 inhibitory effect Effects 0.000 claims description 3
- 235000012736 patent blue V Nutrition 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 2
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 6
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 abstract 1
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
- 239000003242 anti bacterial agent Substances 0.000 description 5
- 239000002244 precipitate Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 241000588724 Escherichia coli Species 0.000 description 2
- -1 Silver ions Chemical class 0.000 description 2
- 238000012512 characterization method Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 238000001856 aerosol method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000002815 broth microdilution Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G5/00—Compounds of silver
- C01G5/02—Halides
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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Abstract
The invention discloses a square AgCl nanoparticle and a preparation method and application thereof. The silver nitrate/nano-material composite material is obtained by compounding silver nitrate and a two-dimensional nano-material, wherein the two-dimensional nano-material is obtained by dispersing a three-dimensional van der waals complex in a solvent for ultrasonic stripping, and the structural formula of the three-dimensional van der waals complex is NiCl2(pyrazine)2(ii) a The square AgCl nanoparticles have the size of about 300-400nm, are square in shape, uniform in shape and difficult to agglomerate. The square AgCl nano-particles have the size of about 300-400nm, uniform appearance, difficult agglomeration and antibacterial aspectShows great application prospect.
Description
Technical Field
The invention relates to AgCl nanoparticles, a preparation method and application thereof, in particular to square AgCl nanoparticles and a preparation method and application thereof.
Background
The silver-based antibacterial agent has a long application history and plays a great role in human health. Silver ions have a strong bactericidal action and even at very low concentrations, they have a significant bacteriostatic action, so that Ag is used in many fields, in particular in medicine+Is widely used as an inorganic antibacterial material. Due to the AgCl energy bandwidth of 3.3eV, under the excitation of near ultraviolet light, electrons can jump from a valence band to a conduction band to form a hole and electron pair, oxygen in water and air is activated, and hydroxyl radical OH and active oxygen ion O are generated2-Both of them have strong oxidizing power, and can destroy the proliferation capacity of bacteria in a short time to make the cells die, thereby achieving the purpose of antibiosis. And researches show that the nano-scale silver-based antibacterial agent has better antibacterial effect than the common silver-based antibacterial agent (environ. Sci. Technol.2010,44,13,5210-5215), and the nano-scale antibacterial agent is a necessary approach for achieving the purpose of practical application. The factors such as the nano-mode and the nano-scale size have important influence on the performance of the material.
The nano material has unique physical and chemical properties due to the size and shape of the nano material. These properties make them suitable for use in a variety of biomedical applications, including cell imaging, drug delivery, and biosensors. To facilitate the use of nanoparticles, researchers are continually searching for new synthetic strategies, and the common method of producing nanoparticles is chemical reduction, and other techniques include ultraviolet radiation, aerosol methods, photolithography, laser ablation, and photochemical reduction. However, these methods are complex and may lead to a variety of nanoparticle morphologies. The application of the two-dimensional nano material technology to the preparation of the silver nano material is an effective solution. In the research field of silver nano materials, the research on preparing the nano AgCl by using the two-dimensional nano materials is not reported yet.
Disclosure of Invention
The technical problem is as follows: in order to solve the practical application of the existing AgCl nanoparticles, the invention provides a square AgCl nanoparticle and a preparation method thereof in a first aspect, wherein the square AgCl nanoparticle is obtained by compounding silver nitrate and a two-dimensional nanomaterial, the two-dimensional nanomaterial is obtained by dispersing a three-dimensional van der Waals complex in a solvent and carrying out ultrasonic stripping, and the structural formula of the three-dimensional van der Waals complex is NiCl2(pyrazine)2(ii) a The second aspect of the invention provides an antibacterial application of the square AgCl nanoparticles prepared by the method; the particle size is about 400nm, the appearance is square, the appearance is uniform, and agglomeration is not easy.
The technical scheme is as follows: the square AgCl nanoparticle is obtained by compounding silver nitrate and a two-dimensional nano material, wherein the two-dimensional nano material is obtained by dispersing a three-dimensional van der Waals complex in a solvent and carrying out ultrasonic stripping, and the structural formula of the three-dimensional van der Waals complex is NiCl2(pyrazine)2(ii) a The square AgCl nanoparticles have the size of about 300-400nm, are square in shape, uniform in shape and difficult to agglomerate.
The preparation method of the square AgCl nano-particles comprises the following steps:
s1, dispersing the three-dimensional van der Waals complex in water, and performing ultrasonic treatment for 30-90min at the temperature of 30-60 ℃ and the frequency of 20-60 kHz;
s2, stirring the solution obtained in the step S1 at 500rpm of 100-;
s3, freeze-drying the Tyndall solution obtained in the step S2 to obtain a two-dimensional nano material;
s4, dispersing the two-dimensional nano material in water, and stirring for 20-60min to obtain a two-dimensional nano material dispersion liquid;
s5, dissolving silver nitrate in water, and adding a surfactant;
and S6, mixing the silver nitrate solution added with the surfactant obtained in the step S5 with the two-dimensional nano material dispersion liquid obtained in the step S4, stirring for 3 hours, filtering, cleaning and precipitating to obtain the square AgCl nano particles.
Wherein,
the ratio of the water to the two-dimensional nano material in the step S1 is 20-100ml:5-25 mg.
In the step S5, the ratio of the water to the silver nitrate is 5-25ml to 2-10mg, and the ratio of the two-dimensional nano material to the silver nitrate is 5-25mg to 2-10 mg. The surfactant is polyvinylpyrrolidone, the molecular weight is 24000-40000, and the added mass is 20-100 mg.
In the step S6, the mixing method is to slowly drop the silver nitrate solution obtained in the step S5 into the two-dimensional nanomaterial dispersion liquid obtained in the step S4, and the stirring speed is 500-1000 rpm.
The preparation steps of the three-dimensional van der waals complex are as follows: mixing NiCl2·6H2Mixing the O aqueous solution and the acetone solution of pyrazine to separate out sky blue solid, stirring the suspension for 0.5-1h, filtering, cleaning and precipitating to obtain the three-dimensional van der Waals complex NiCl2(pyrazine)2。
The ratio of the three-dimensional van der Waals complex to the solvent in step S1 is 10-30mg:50-100 mL.
The application of the square AgCl nano-particles is as follows: can be used for inhibiting growth of Escherichia coli and microorganism.
Has the advantages that: the square AgCl nano-particles prepared by the invention have the following advantages:
(1) the purity is high and the size is uniform;
(2) the dispersion agent exists stably in both solution and solid states, has good dispersion, is not easy to agglomerate and has stable performance;
(3) the preparation method is simple and easy to operate;
(4) can be used for preparing antibacterial agent.
Drawings
FIG. 1 is a three-dimensional van der Waals complex NiCl2(pyrazine)2A schematic of the crystal structure of (a);
FIG. 2 is a scanning electron microscope image of square AgCl nanoparticles prepared by the present invention.
Detailed Description
Example 1
Three-dimensional van der Waals complex NiCl2(pyrazine)2Synthesis of
1.0mmol of NiCl2·6H2O and 2.0mmol of pyrazine were dissolved in 10ml of water and 5ml of acetone, respectively, and the acetone solution of pyrazine was slowly added dropwise to NiCl2Gradually separating out sky blue solid precipitate in the aqueous solution, stirring for 0.5-1h, filtering, washing the precipitate with 10ml acetone, and vacuum drying to obtain the three-dimensional van der Waals complex NiCl2(pyrazine)2. The crystal structure is shown in figure 1.
Two-dimensional nanomaterial preparation
Three-dimensional Van der Waals complex NiCl prepared as in example 12(pyrazine)2The method is used for preparing the two-dimensional nano material and comprises the following specific steps:
s1, mixing 10mg of three-dimensional Van der Waals complex NiCl2(pyrazine)2Dispersing the mixture in 50mL of aqueous solvent in a 100mL beaker, and carrying out ultrasonic treatment for 60min at 30 ℃ and 40 kHz;
s2, stirring the solution obtained in the step S1 at 500rpm for 12 hours, standing for 24 hours, centrifuging at 3000rpm to remove precipitates to obtain a Tyndall solution with good dispersibility;
s3, freeze-drying the Tyndall solution to obtain a light green two-dimensional nano material; the thickness was 2nm and the lateral dimension was 1 μm. The two-dimensional nanomaterial morphology is shown in figure 2.
Preparation of square AgCl nanoparticles
The two-dimensional nanomaterial prepared in example 2 was used to prepare square AgCl nanoparticles, with the following specific steps:
(1) 5mg of two-dimensional nanomaterial was dispersed in 20ml of water and stirred for 30 min.
(2) 2mg of silver nitrate are dissolved in 5ml of water, and polyvinylpyrrolidone of molecular weight 40000 is added in an amount of 20 mg.
(3) And (3) slowly dropwise adding the silver nitrate solution obtained in the step (2) into the two-dimensional nano material dispersion liquid obtained in the step (1), stirring at a stirring speed of 1000rpm for 3 hours, and repeatedly centrifuging, cleaning and precipitating to obtain the square AgCl nano particles.
Two-dimensional nanomaterial morphology characterization
The appearance of the ultrathin two-dimensional spin-crossover nanomaterial prepared in example 2 is characterized by a transmission electron microscope, and fig. 2 shows a TEM image of the two-dimensional nanomaterial at a scale of 1 μm, and the image clearly shows a bulk ultrathin film.
Square AgCl nanoparticle morphology characterization
The morphology of the AgCl nanoparticles prepared in example 3 was characterized by scanning electron microscopy.
AgCl nanoparticle antibacterial experiment
The Minimum Inhibitory Concentration (MIC) of AgCl nanoparticles against e.coli was determined using broth dilution. The measurement result shows that: the MIC of the conventional AgCl nanoparticles was 0.625mg/L, while the MIC of the square AgCl nanoparticles of the present invention was 0.078 mg/L. These results show that the square AgCl nanoparticles obtained by the method have better superiority in sterilization.
Claims (8)
1. The square AgCl nanoparticle is characterized by being obtained by compounding silver nitrate and a two-dimensional nano material, wherein the two-dimensional nano material is obtained by dispersing a three-dimensional van der Waals complex in a solvent and carrying out ultrasonic stripping, and the structural formula of the three-dimensional van der Waals complex is NiCl2(pyrazine)2(ii) a The square AgCl nanoparticles have the size of about 300-400nm, are square in shape, uniform in shape and difficult to agglomerate.
2. A method of preparing square AgCl nanoparticles according to claim 1, wherein the square AgCl nanoparticles are prepared by the steps of:
s1, dispersing the three-dimensional van der Waals complex in water, and performing ultrasonic treatment for 30-90min at the temperature of 30-60 ℃ and the frequency of 20-60 kHz;
s2, stirring the solution obtained in the step S1 at 500rpm of 100-;
s3, freeze-drying the Tyndall solution obtained in the step S2 to obtain a two-dimensional nano material;
s4, dispersing the two-dimensional nano material in water, and stirring for 20-60min to obtain a two-dimensional nano material dispersion liquid;
s5, dissolving silver nitrate in water, and adding a surfactant;
and S6, mixing the silver nitrate solution added with the surfactant obtained in the step S5 with the two-dimensional nano material dispersion liquid obtained in the step S4, stirring for 3 hours, filtering, cleaning and precipitating to obtain the square AgCl nano particles.
3. The method for preparing square AgCl nanoparticles of claim 2, wherein the ratio of water to two-dimensional nanomaterial in step S1 is 20-100ml:5-25 mg.
4. The preparation method of square AgCl nanoparticles as claimed in claim 2, wherein the ratio of water to silver nitrate in step S5 is 5-25ml:2-10mg, and the ratio of two-dimensional nanomaterial to silver nitrate is 5-25mg:2-10 mg. The surfactant is polyvinylpyrrolidone, the molecular weight is 24000-40000, and the added mass is 20-100 mg.
5. The method for preparing square AgCl nanoparticles as claimed in claim 2, wherein the mixing in step S6 is performed by slowly dropping the silver nitrate solution obtained in step S5 into the two-dimensional nanomaterial dispersion obtained in step S4 at a stirring speed of 500-1000 rpm.
6. The method of preparing square AgCl nanoparticles according to claim 2, wherein the three-dimensional van der waals complex is prepared by: mixing NiCl2·6H2Mixing the O aqueous solution and the acetone solution of pyrazine to separate out sky blue solid, stirring the suspension for 0.5-1h, filtering, cleaning and precipitating to obtain the three-dimensional van der Waals complex NiCl2(pyrazine)2。
7. The method for preparing square AgCl nanoparticles as claimed in claim 2, wherein the ratio of the three-dimensional van der waals complex to the solvent in step S1 is 10-30mg:50-100 mL.
8. Use of square AgCl nanoparticles according to claim 1 for inhibiting the growth of e.
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| CN111153428A (en) * | 2020-01-19 | 2020-05-15 | 东南大学 | Preparation method and application of square AgCl nanoparticles |
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| CN105498844A (en) * | 2015-12-07 | 2016-04-20 | 辽宁师范大学 | In-situ preparation method and application of Ag/AgCl/NH2-MIL-101(Fe) composite photocatalyst with spindle appearance |
| CN108864206A (en) * | 2018-07-25 | 2018-11-23 | 东南大学 | A kind of ultra-thin two-dimension spin crossover nano material and its preparation method and application |
| CN108918855A (en) * | 2018-07-31 | 2018-11-30 | 济南大学 | A kind of preparation method and application based on signal " on-off " type Electrochemiluminescsensor sensor that AgNCs is illuminator |
| CN110085446A (en) * | 2019-04-11 | 2019-08-02 | 北京工业大学 | A kind of preparation method of original position Ni doping Co-MOF-74 electrode material for super capacitor |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105498844A (en) * | 2015-12-07 | 2016-04-20 | 辽宁师范大学 | In-situ preparation method and application of Ag/AgCl/NH2-MIL-101(Fe) composite photocatalyst with spindle appearance |
| CN108864206A (en) * | 2018-07-25 | 2018-11-23 | 东南大学 | A kind of ultra-thin two-dimension spin crossover nano material and its preparation method and application |
| CN108918855A (en) * | 2018-07-31 | 2018-11-30 | 济南大学 | A kind of preparation method and application based on signal " on-off " type Electrochemiluminescsensor sensor that AgNCs is illuminator |
| CN110085446A (en) * | 2019-04-11 | 2019-08-02 | 北京工业大学 | A kind of preparation method of original position Ni doping Co-MOF-74 electrode material for super capacitor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111153428A (en) * | 2020-01-19 | 2020-05-15 | 东南大学 | Preparation method and application of square AgCl nanoparticles |
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