CN103480858A - Silver nano particle preparation method using visible light to reduce silver ions - Google Patents
Silver nano particle preparation method using visible light to reduce silver ions Download PDFInfo
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- CN103480858A CN103480858A CN201310429586.9A CN201310429586A CN103480858A CN 103480858 A CN103480858 A CN 103480858A CN 201310429586 A CN201310429586 A CN 201310429586A CN 103480858 A CN103480858 A CN 103480858A
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- silver
- nano
- visible light
- particles
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 13
- 239000004332 silver Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000002105 nanoparticle Substances 0.000 title abstract description 3
- -1 silver ions Chemical class 0.000 title abstract 3
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 13
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 9
- 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 claims abstract description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 14
- 238000005119 centrifugation Methods 0.000 claims description 8
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 7
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 claims description 3
- 229940071536 silver acetate Drugs 0.000 claims description 3
- OQXSRALAOPBHPM-UHFFFAOYSA-N 2-hydroxypropanoic acid;silver Chemical compound [Ag].CC(O)C(O)=O OQXSRALAOPBHPM-UHFFFAOYSA-N 0.000 claims description 2
- 230000005855 radiation Effects 0.000 claims description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 230000000844 anti-bacterial effect Effects 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 30
- 241000976924 Inca Species 0.000 description 6
- 238000005259 measurement Methods 0.000 description 6
- 238000006722 reduction reaction Methods 0.000 description 5
- 229940083025 silver preparation Drugs 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000003223 protective agent Substances 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 239000003021 water soluble solvent Substances 0.000 description 1
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Abstract
The invention discloses a silver nano particle preparation method using visible light to reduce silver ions. The method includes: adding soluble silver salt into 5-10mg/L methylene blue solution, stirring for 20-80 hours under irradiation of sunlight or artificial visible light to reduce silver ions into nano silver, centrifugally separating, and drying to obtain silver nano particles. The method is simple in process, low in cost, and the like, the prepared silver nano particles are applicable to fields such as industrial catalysis and antibacterial materials.
Description
(1) technical field:
The present invention relates to a kind of visible ray reducing metal ion and prepare the nano particle method, mainly relate to a kind of visible ray reduction silver ion and prepare the silver nano-grain method.
(2) background technology:
Nano-Ag particles, owing to having catalysis, the performance such as antibiotic, therefore, is usually used in the numerous areas such as antiseptic and industrial catalyst.In recent years; the technology of preparing of nano-Ag particles is one of focus of the subject researchs such as materialogy, chemistry; Chinese patent (CN101966595A) discloses a kind of nano silver preparation process; process is that silver salt and protective agent are dissolved in water-soluble solvent or alcohols solvent; regulate the pH value, make the value range of pH value in needs, then add reducing agent; heating stirring reaction 20-30 minute, obtain golden yellow Nano silver solution.PH value owing to needing regulator solution in the Nano Silver preparation process, also will add protective agent, reducing agent etc., and preparation process is comparatively loaded down with trivial details, and cost is higher.
(3) summary of the invention:
The object of the present invention is to provide a kind of visible ray reduction silver ion to prepare the nano-Ag particles method, nano-Ag particles can be for Industrial Catalysis, the numerous areas such as antibiotic.
The object of the present invention is achieved like this:
The silver salt of solubility being joined in the 5-100mg/L methylene blue solution, then under sunshine or artificial visible ray, stir 20-80 hour, can be Nano Silver by silver ion reduction, after centrifugation, drying, is prepared into silver nano-grain.
Wherein the silver salt of solubility and methylene blue solution mass ratio are 1: 20-1: 500.
Wherein the silver salt of solubility refers in silver nitrate, silver acetate, actol a kind of.
The present invention mainly utilizes the photoactivate performance of methylene blue solution, under radiation of visible light, can produce active oxygen, and active oxygen prepares silver nano-grain by the silver ion photo-reduction.With existing Nano Silver preparation method, compare, this kind of method has that preparation technology is simple, low cost and other advantages, can be widely used in wastewater treatment, metal nano material and the numerous areas such as prepare, and has a extensive future.
(4) accompanying drawing explanation: Fig. 1 is that a kind of visible ray reduction silver ion of the present invention prepares the prepared nano-Ag particles scanning electron microscope (SEM) photograph of nano-Ag particles method.
(5) specific embodiment:
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment mono-
The methylene blue solution that adds 1 gram silver nitrate and 500 milliliters, 5mg/L in beaker, be placed under the 40W fluorescent lamp and stir 50 hours, after then centrifugation, drying, can be prepared into 0.12 gram nano-Ag particles.Measurement result: adopt INCA type X-ray energy spectrometer to analyze the composition of particle, by the JSM-6700F of company of NEC scanning electron microscopic observation the nano-Ag particles pattern, result shows: as seen from Figure 1, prepared particle is elemental silver nanoparticles, and granular size is between 5-100nm.
Embodiment bis-
Add in beaker in the methylene blue solution of 1 gram silver nitrate and 20 milliliters, 100mg/L, be placed under sunshine and stir 80 hours, after then centrifugation, drying, can be prepared into 0.18 gram nano-Ag particles.Measurement result: adopt INCA type X-ray energy spectrometer to analyze the composition of particle, by the JSM-6700F of company of NEC scanning electron microscopic observation the nano-Ag particles pattern, result shows: prepared particle is elemental silver nanoparticles, and granular size is between 15-150nm.
Embodiment tri-
Add in beaker in the methylene blue solution of 1 gram silver nitrate and 200 milliliters, 80mg/L, be placed in the lower stirring of 100W incandescent lamp 20 hours, after then centrifugation, drying, can be prepared into 0.10 gram nano-Ag particles.Measurement result: adopt INCA type X-ray energy spectrometer to analyze the composition of particle, by the JSM-6700F of company of NEC scanning electron microscopic observation the nano-Ag particles pattern, result shows: prepared particle is elemental silver nanoparticles, and granular size is between 5-90nm.
Embodiment tetra-
Add in beaker in the methylene blue solution of 1 gram silver acetate and 500 milliliters, 10mg/L, be placed under sunshine and stir 30 hours, after then centrifugation, drying, can be prepared into 0.13 gram nano-Ag particles.Measurement result: adopt INCA type X-ray energy spectrometer to analyze the composition of particle, by the JSM-6700F of company of NEC scanning electron microscopic observation the nano-Ag particles pattern, result shows: prepared particle is elemental silver nanoparticles, and granular size is between 10-120nm.
Embodiment five
Add in beaker in the methylene blue solution of 1 gram silver nitrate and 400 milliliters, 10mg/L, be placed under sunshine and stir 60 hours, after then centrifugation, drying, can be prepared into 0.17 gram nano-Ag particles.Measurement result: adopt INCA type X-ray energy spectrometer to analyze the composition of particle, by the JSM-6700F of company of NEC scanning electron microscopic observation the nano-Ag particles pattern, result shows: prepared particle is elemental silver nanoparticles, and granular size is between 10-130nm.
Embodiment six
Add in beaker in the methylene blue solution of 1 gram silver nitrate and 300 milliliters, 20mg/L, be placed under the 100W incandescent lamp and stir 50 hours, after then centrifugation, drying, can be prepared into 0.15 gram nano-Ag particles.Measurement result: adopt INCA type X-ray energy spectrometer to analyze the composition of particle, by the JSM-6700F of company of NEC scanning electron microscopic observation the nano-Ag particles pattern, result shows: prepared particle is elemental silver nanoparticles, and granular size is between 10-120nm.
Claims (3)
1. a visible ray reduction silver ion prepares the silver nano-grain method, the steps include:
Soluble silver salt being joined in the 5-100mg/L methylene blue solution, then under sunshine or artificial radiation of visible light, stir 20-80 hour, can be Nano Silver by silver ion reduction, after centrifugation, drying, is prepared into silver nano-grain.
2. a kind of visible ray reduction silver ion according to claim 1 prepares the silver nano-grain method, and wherein soluble silver salt and methylene blue solution mass ratio are 1: 20-1: 500.
3. a kind of visible ray reduction silver ion according to claim 1 prepares the silver nano-grain method, and wherein the silver salt of solubility refers to a kind of in silver nitrate, silver acetate, actol.
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| CN201310429586.9A CN103480858B (en) | 2013-09-10 | 2013-09-10 | Silver nano particle preparation method using visible light to reduce silver ions |
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| CN201310429586.9A CN103480858B (en) | 2013-09-10 | 2013-09-10 | Silver nano particle preparation method using visible light to reduce silver ions |
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| CN103480858B CN103480858B (en) | 2015-05-06 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103894625A (en) * | 2014-04-21 | 2014-07-02 | 中国医学科学院生物医学工程研究所 | Preparation method for bionic nano-silver |
| CN104308184A (en) * | 2014-10-24 | 2015-01-28 | 武汉理工大学 | Method for preparing Au-Ag (gold-silver) nuclear shell nano particles by visible light |
| CN105014093A (en) * | 2015-01-09 | 2015-11-04 | 宁波工程学院 | Preparation method for carbon nanoparticles with visible light loaded with Pt |
| CN105798328A (en) * | 2016-05-18 | 2016-07-27 | 深圳市国华光电科技有限公司 | Silver nanoparticle preparation method |
| CN113265164A (en) * | 2021-06-08 | 2021-08-17 | 绵竹市天使农业科技有限公司 | Preparation method of environment-friendly health-care coating |
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| JP2005220435A (en) * | 2003-10-22 | 2005-08-18 | Mitsuboshi Belting Ltd | Method of producing metal nanoparticle and dispersion of metal nanoparticle |
| CN101306468A (en) * | 2007-05-19 | 2008-11-19 | 浙江师范大学 | Preparation method of conductive polypyrrole-wrapped copper-silver composite nanoparticles |
| US20110017019A1 (en) * | 2008-04-28 | 2011-01-27 | Tata Chemicals Limited | Process for the preparation of silver nano particles |
| CN102581299A (en) * | 2012-02-21 | 2012-07-18 | 金淞电器(九江)有限公司 | Photochemical preparation method of noble metal nanoparticles |
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2013
- 2013-09-10 CN CN201310429586.9A patent/CN103480858B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20030136223A1 (en) * | 2001-09-26 | 2003-07-24 | Rongchao Jin | Nanoprisms and method of making them |
| JP2005220435A (en) * | 2003-10-22 | 2005-08-18 | Mitsuboshi Belting Ltd | Method of producing metal nanoparticle and dispersion of metal nanoparticle |
| CN1569369A (en) * | 2004-05-12 | 2005-01-26 | 北京科技大学 | Industrialized preparation technology of nm-class silver powder |
| CN101306468A (en) * | 2007-05-19 | 2008-11-19 | 浙江师范大学 | Preparation method of conductive polypyrrole-wrapped copper-silver composite nanoparticles |
| US20110017019A1 (en) * | 2008-04-28 | 2011-01-27 | Tata Chemicals Limited | Process for the preparation of silver nano particles |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103894625A (en) * | 2014-04-21 | 2014-07-02 | 中国医学科学院生物医学工程研究所 | Preparation method for bionic nano-silver |
| CN103894625B (en) * | 2014-04-21 | 2016-09-21 | 中国医学科学院生物医学工程研究所 | A kind of preparation method of bionic nano silver |
| CN104308184A (en) * | 2014-10-24 | 2015-01-28 | 武汉理工大学 | Method for preparing Au-Ag (gold-silver) nuclear shell nano particles by visible light |
| CN104308184B (en) * | 2014-10-24 | 2016-08-24 | 武汉理工大学 | A kind of visible ray prepares the method for Au-Ag core-shell nano |
| CN105014093A (en) * | 2015-01-09 | 2015-11-04 | 宁波工程学院 | Preparation method for carbon nanoparticles with visible light loaded with Pt |
| CN105798328A (en) * | 2016-05-18 | 2016-07-27 | 深圳市国华光电科技有限公司 | Silver nanoparticle preparation method |
| CN105798328B (en) * | 2016-05-18 | 2018-01-30 | 深圳市国华光电科技有限公司 | The preparation method of silver nano-grain |
| CN113265164A (en) * | 2021-06-08 | 2021-08-17 | 绵竹市天使农业科技有限公司 | Preparation method of environment-friendly health-care coating |
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Effective date of registration: 20180426 Address after: 246123 Jinan town Industrial Park, Huaining, Anqing, Anhui Patentee after: Anhui thriving Packing Co., Ltd. Address before: 246003 College of resources and environment, Anqing Teachers College, 128 Linghu South Road, Anqing, Anhui Patentee before: Xu Zhibing |