CN102728850B - Method for preparing high-stability polymer coated nano silver cluster - Google Patents

Method for preparing high-stability polymer coated nano silver cluster Download PDF

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Publication number
CN102728850B
CN102728850B CN201210205773.4A CN201210205773A CN102728850B CN 102728850 B CN102728850 B CN 102728850B CN 201210205773 A CN201210205773 A CN 201210205773A CN 102728850 B CN102728850 B CN 102728850B
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cluster
polymer
nano
nano silver
silane
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CN102728850A (en
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何瑜
王仁宗
宋功武
朱晶晶
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Hubei University
Hubei Forbon Technology Co Ltd
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Hubei University
Hubei Forbon Technology Co Ltd
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Abstract

The invention discloses a method for preparing a high-stability polymer coated a nano silver cluster, and is characterized by comprising the following steps of: (1) synthesizing a silane-Ag complex, namely dissolving 0.0370 to 0.0986 gram of silver nitrate in 10 to 30 milliliters of absolute methanol, adding 200 to 600 mu litters of silane, and stirring in a dark place for 1 to 4 hours; (2) synthesizing a polymer-modified nano silver cluster, namely dissolving 0.0363 to 0.0968 gram of polymer in 1 to 20 milliliters of water, adding solution formed by the step (1), stirring for 1 to 30 minutes; and (3) adding 10 to 100 mu liters of absolute formaldehyde, stirring in a dark place for 3 to 6 hours, obtaining a yellow solution, settling and filtering to obtain the polymer-modified nano silver cluster. The polymer-modified nano silver cluster synthesized by the method has the advantages of low price, stable performance, no toxicity and the like. The cluster has very high practical value and has a great prospect in environment analysis, biochemical analysis, food safety and other fields.

Description

The ag nano-cluster preparation method of high stability polymer wrapped
Technical field:
The invention belongs to field of nano material preparation, relate to a kind of ag nano-cluster preparation method of high stability polymer wrapped.
Background technology:
Cluster forms metastable aggregation by physics and chemistry adhesion by several to several thousand atoms, molecule, ions, its bulk at several dusts to the scope of hundreds of dust.Because cluster size is special, it has a series of single atom, molecules of being different from, also the physical property and the chemical property that are different from bulk solid material, have the quantum size effect of abnormal high chemism and catalytic performance, light and physical dimension effect that nonlinear effect, electricity are led, adulterate and mix the electric conductivity etc. of the electric conductivity of bag atom and superconductivity, carbon pipe, carbon green onion as great specific surface makes it.
In recent years, noble metal (gold, silver) nanocluster is because quantum size effect, small-size effect show desirable optics and electric property becomes one of the focus in nano materials research field.When nanoparticle size be reduced to gradually when suitable with Fermi's wavelength (<0.5 nm) can present with semiconductor type like feature, produce the separated and emitting fluorescence of energy level.For traditional fluorescent marker, ag nano-cluster has many advantages.Organic fluorescent dye easily produces photobleaching; Semiconductor nanoparticle preparation condition is harsh, and material toxicity is large; And ag nano-cluster just can synthesize under condition as mild as a dove, and glow color is adjustable with cluster size, as a kind of potential fluorescent marker, is expected to be applied to the fields such as photoimaging, biomarker, chemical sensor.
In addition, what research was both at home and abroad more at present is gold nano cluster, and ag nano-cluster is because its stability is difficult to control thereby limited its development.Secondly, the dressing agent of preparing the selection of gold and silver nanocluster is also mostly the reagent that this class of DNA is comparatively expensive, and cost is higher.
Summary of the invention:
For the existing problem and shortage of prior art, the present invention aims to provide a kind of ag nano-cluster preparation method of simple stable high stability polymer wrapped.That the method has is simple to operate, low price, stable performance, the advantage such as nontoxic, and instrument equipment is conventional equipment, as: magnetic stirring apparatus, round-bottomed flask etc.The ag nano-cluster stable performance of preparation, be easy to preserve.
The ag nano-cluster preparation method of high stability polymer wrapped, is characterized in that comprising the following steps:
(1) silane-Ag complex compound is synthetic: take 0.0370~0.0986 g silver nitrate and be dissolved in 10~30 ml absolute methanols, then add wherein 200~600 uL silane, 1~4h is stirred in dark place;
(2) polymer-modified ag nano-cluster is synthetic: take 0.0363~0.0968 g polymer and be dissolved in 1~20 ml water, add in the solution of step (1), stir 1~30 min; Add 10~100 uL anhydrous formaldehydes again, continue dark place and stir 3~6 h, obtain yellow solution, sedimentation and filtration obtains polymer-modified ag nano-cluster.
Silane in described step (1) is 3-aminopropyl triethoxysilane (APTES), 3-(2-aminoethyl) aminopropyl trimethoxysilane (APTMOS) or 4-ammonia butyl trimethoxy silane.
Polymer in described step (2) is polymine (PEI), polyamide-amide type dendrimer (PAMAM) or PMA (PMAA).
The polymer-modified ag nano-cluster that the present invention synthesizes has low price, stable performance, the advantage such as nontoxic, has very high practical value, in fields such as environmental analysis, biochemical analysis, food securities, has comparatively wide application prospect.
Accompanying drawing explanation:
Fig. 1 is the TEM figure of the ag nano-cluster of the present embodiment 1.
Fig. 2 is the TEM figure of the ag nano-cluster of the present embodiment 2.
Fig. 3 is the TEM figure of the ag nano-cluster of the present embodiment 3.
The specific embodiment:
Below in conjunction with specific embodiment, the invention will be further described, but the present invention is not limited to following examples.
Embodiment 1:
1) silane-Ag complex compound is synthetic: first, take 0.0370 g silver nitrate and be dissolved in 20 ml methyl alcohol, then add wherein 200 uL 3-aminopropyl triethoxysilane APTES, 1 h is stirred in dark place;
2), in solution synthesizing of polymer-modified ag nano-cluster: take 0.0363 g polymine PEI and be dissolved in 1ml water, add step 1), stir 3 min; Add 40 uL anhydrous formaldehydes again, continue dark place and stir 6 h, obtain yellow-brownish solution, sedimentation and filtration obtains polymer-modified ag nano-cluster, and the TEM figure of polymer-modified ag nano-cluster as shown in Figure 1.
3) get the ag nano-cluster of preparation for the detection of Hg, detect be limited to 0.1 nanomole/liter.
Embodiment 2:
1) silane-Ag complex compound is synthetic: first, take 0.0616 g silver nitrate and be dissolved in 30 ml methyl alcohol, then add wherein 338 uL 3-(2-aminoethyls) aminopropyl trimethoxysilane APTMOS, 2 h are stirred in dark place;
2), in solution synthesizing of polymer-modified ag nano-cluster: take 0.0605 polyamide-amide type dendrimer PAMAM and be dissolved in 20 ml water, add step 1), stir 1 min; Add 10 uL anhydrous formaldehydes again, continue dark place and stir 5 h, obtain yellow solution, sedimentation and filtration obtains polymer-modified ag nano-cluster, and the TEM figure of polymer-modified ag nano-cluster as shown in Figure 2.
3) get the ag nano-cluster of preparation for the detection of Hg, detect be limited to 0.1 nanomole/liter.
Embodiment 3:
1) silane-Ag complex compound is synthetic: first, take 0.0986 g silver nitrate and be dissolved in 10 ml methyl alcohol, then add wherein 600uL 4-ammonia butyl trimethoxy silane, 4h is stirred in dark place;
2), in solution synthesizing of polymer-modified ag nano-cluster: take 0.0968 g PMA PMAA and be dissolved in 15 ml water, add step 1), stir 30 min; Add 100uL formaldehyde again, continue dark place and stir 3h, obtain yellow solution, sedimentation and filtration obtains polymer-modified ag nano-cluster, and the TEM figure of polymer-modified ag nano-cluster as shown in Figure 3.
3) get the ag nano-cluster of preparation for the detection of Hg, detect be limited to 0.1 nanomole/liter.

Claims (1)

1. the ag nano-cluster preparation method of high stability polymer wrapped, is characterized in that comprising the following steps:
(1) silane-Ag complex compound is synthetic: take 0.0370~0.0986 g silver nitrate and be dissolved in 10~30 ml absolute methanols, then add wherein 200~600 uL silane, 1~4h is stirred in dark place; Described silane is 3-aminopropyl triethoxysilane (APTES),
(2) polymer-modified ag nano-cluster is synthetic: take 0.0363~0.0968 g polymer and be dissolved in 1~20 ml water, add in the solution of step (1), stir 1~30 min; Add 10~100 uL anhydrous formaldehydes again, continue dark place and stir 3~6 h, obtain yellow solution, sedimentation and filtration obtains polymer-modified ag nano-cluster; Described polymer is polymine (PEI).
CN201210205773.4A 2012-06-20 2012-06-20 Method for preparing high-stability polymer coated nano silver cluster Expired - Fee Related CN102728850B (en)

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CN103624268B (en) * 2013-11-13 2016-06-29 苏州大学 The preparation method of the sugary ag nano-cluster of anticancer fluorescence
CN104722779B (en) * 2013-12-23 2017-05-10 华东理工大学 Silver nanocluster preparation method with hydrogen serving as reducing agent
CN103990811B (en) * 2014-05-30 2015-11-18 吉林大学 Electropositive metal fluorescence nano point, preparation method and the application in cell fluorescence imaging thereof
TWI580644B (en) * 2015-04-27 2017-05-01 楊謹瑋 Nano silver preparation method and application thereof
CN109438699B (en) * 2018-09-26 2022-01-11 上海维凯光电新材料有限公司 Modified polyethyleneimine/nano-silver composite material and preparation method thereof
CN112480595A (en) * 2020-12-05 2021-03-12 勇气模具塑胶(苏州)有限公司 Composite material for refrigerator partition plate and preparation method thereof

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CN101107257A (en) * 2005-02-07 2008-01-16 印可得株式会社 Organic silver complexes, their preparation methods and their methods for forming thin layers
CN101951968A (en) * 2007-10-08 2011-01-19 庄臣及庄臣视力保护公司 Methods for forming stabilized metal salt particles
CN102218544A (en) * 2011-05-27 2011-10-19 中国科学院理化技术研究所 Preparation method and application of metal nanoparticles

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Publication number Priority date Publication date Assignee Title
CN101107257A (en) * 2005-02-07 2008-01-16 印可得株式会社 Organic silver complexes, their preparation methods and their methods for forming thin layers
CN101951968A (en) * 2007-10-08 2011-01-19 庄臣及庄臣视力保护公司 Methods for forming stabilized metal salt particles
CN102218544A (en) * 2011-05-27 2011-10-19 中国科学院理化技术研究所 Preparation method and application of metal nanoparticles

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