CN1899733A - New method for preparing functional metal nano particles - Google Patents
New method for preparing functional metal nano particles Download PDFInfo
- Publication number
- CN1899733A CN1899733A CN 200610047260 CN200610047260A CN1899733A CN 1899733 A CN1899733 A CN 1899733A CN 200610047260 CN200610047260 CN 200610047260 CN 200610047260 A CN200610047260 A CN 200610047260A CN 1899733 A CN1899733 A CN 1899733A
- Authority
- CN
- China
- Prior art keywords
- organic
- water
- nano particles
- preparing functional
- metal nano
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention belongs to the field of nano material preparing technology in material chemistry, and is especially process of preparing functional nanometer metal particle. The process of preparing functional nano metal particle includes the following steps: 1. dissolving organic protecting reagent and organic reducing agent in water insoluble organic solvent at 10-200deg.c, with the dissolved organic protecting reagent and organic reducing agent having concentration of 1-50 % each; 2. dissolving water soluble metal salt in water at 10-200deg.c in the concentration of 0.1-50 %; and 3. mixing the water phase and the organic phase in the volume ratio of 1 to 1-100, reacting at 10-200deg.c for 1-24 hr and separating out the organic phase to obtain organic solution of functional nanometer metal. The prepared functional nanometer metal particle has high dispersivity and high stability.
Description
Technical field
The invention belongs to the nano material preparation technical field in the materials chemistry.Relate to a kind of method for preparing the metal nanoparticle of high dispersive, high stability, specifically a kind of method for preparing functional metal nano particles.
Background technology
The functional metal nano particles of control preparation high dispersive, high stability is important field of research in the nano material preparation.At present, the heterogeneous mixing method preparation of many employings in the document, promptly slaine, reducing agent and protective agent are with going out a reaction medium.The water of reporting in the document-organic two phase process then is that organic metal salt and protective agent are dissolved in organic facies, and reducing agent is soluble in the aqueous phase.And in the present invention, adopting water-organic two-phase method, its innovation part is that reducing agent and protective agent are dissolved in organic facies, and slaine is soluble in the aqueous phase.The functional metal nano particles that utilizes this method to prepare comprises: Pd, Pt, Rh, Ru, Ir, Au, Ag, Co, Ni.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing functional metal nano particles simple to operate.
Technical solution of the present invention is, a kind of new method for preparing functional metal nano particles, its method be, the preparation system is by two phase compositions of water-organic facies, the aqueous phase dissolved metallic salt, and agent of organic facies dissolving and reducing and protection reagent, preparation process is:
A, with organic protection reagent, organic reducing agent is dissolved in the immiscible organic solvent of water in, temperature is 10-200 ℃, the concentration of the organic protection reagent after the dissolving is 1-50%, the concentration of organic reducing agent is 1-50%;
B, the water-soluble metal salt is dissolved in the water, temperature is 10-200 ℃, and the concentration of the slaine after the dissolving is 0.1-50%;
C, under stirring condition, above-mentioned water and organic facies are mixed with 1: 1～1: 100 volume ratio, holding temperature is at 10-200 ℃, react after 1-24 hour, tell the nano metal organic solution that organic facies just can obtain functionalization, metal nanoparticle is: Pd, Pt, Rh, Ru, Ir, Au, Ag, Co, Ni; Described organic facies is meant the organic solvent immiscible with water, comprises cyclohexane, n-hexane, normal heptane, normal octane, positive nonane, n-decane, benzene,toluene,xylene; Described water-soluble metal salt comprises: PdCl
2, PtCl
2, RhCl
3, RuCl
3, HAuCl
4, AgNO
3, Ag (NH
3)
2NO
3, CoNO
3, NiNO
3Described organic protection reagent is organic amine, organic mercaptan and organophosphor; comprise: lauryl amine, tetradecy lamine, cetylamine, octadecylamine, aromatic amine and have substituent aromatic amine; lauryl mercaptan, tetradecanylthioalcohol, 16 mercaptan, stearylmercaptan, aromatic thiol and have substituent aromatic thiol; the organic reagent that contains amido and sulfydryl simultaneously: p-Mercaptoaniline, organophosphor is as triphenyl phosphorus, triethyl phosphine.Described organic reducing agent is organic aldehydes and organic hydrazine class, comprising: formaldehyde, acetaldehyde, propionic aldehyde, benzaldehyde, phenylacetaldehyde, furfural, phenylhydrazine, to procarbazine.Better effects if when the temperature of preparation metal nanoparticle is 20-180 ℃.
The invention has the beneficial effects as follows: preparation process is simple, easy operating and repetition.The functional metal nano particles of preparation has polymolecularity and high stability.
Description of drawings
The invention will be further described below in conjunction with the drawings and specific embodiments.
Fig. 1 is the transmission electron microscope photo of the functionalized nano Au particle of preparation.
Fig. 2 is the transmission electron microscope photo of the functionalized nano Ag particle of preparation.
The specific embodiment
Embodiment 1
1.5 gram lauryl amines are joined in 50 milliliters of cyclohexanes 20 ℃ of stirring and dissolving.And then add 15 milliliter of 37% formalin, and stir after 15 minutes, tell organic layer (cyclohexane layer) with separatory funnel.Under condition of stirring, with 5 milliliters of liquor argenti nitratis ophthalmicus (0.1g AgNO
3) join above-mentioned cyclohexane layer, 20 ℃ were stirred after 30 minutes, and telling the upper strata with separatory funnel again is the cyclohexane layer, can obtain the Nano Silver cyclohexane solution of functionalization.
Embodiment 2
1.5 gram lauryl amines are joined in 50 milliliters of cyclohexanes 20 ℃ of stirring and dissolving.And then add 15 milliliter of 37% formalin, and stir after 15 minutes, tell organic layer (cyclohexane layer) with separatory funnel.Under condition of stirring, with 1 milliliter of HAuCl
4Solution (1g HAuCl
4Be dissolved in 100 ml waters) join above-mentioned cyclohexane layer, 20 ℃ were stirred after 30 minutes, and telling the upper strata with separatory funnel again is the cyclohexane layer, can obtain the nm of gold cyclohexane solution of functionalization.
Embodiment 3
1.5 gram lauryl amines are joined in 30 milliliters of toluene 30 ℃ of stirring and dissolving.And then add 10 milliliters of benzaldehydes, stir after 20 minutes, under condition of stirring, 5 milliliters of liquor argenti nitratis ophthalmicus (0.1g AgNO
3) join above-mentioned toluene solution, 50 ℃ were stirred after 6 hours, and telling the upper strata with separatory funnel again is toluene layer, can obtain the Nano Silver toluene solution of functionalization.
Claims (6)
1, a kind of new method for preparing functional metal nano particles is characterized in that, its method is, the preparation system is by two phase compositions of water-organic facies, the aqueous phase dissolved metallic salt, and agent of organic facies dissolving and reducing and protection reagent, preparation process is:
A, with organic protection reagent, organic reducing agent is dissolved in the immiscible organic solvent of water in, temperature is 10-200 ℃, the concentration of the organic protection reagent after the dissolving is 1-50%, the concentration of organic reducing agent is 1-50%;
B, the water-soluble metal salt is dissolved in the water, temperature is 10-200 ℃, and the concentration of the slaine after the dissolving is 0.1-50%;
C, under stirring condition, above-mentioned water and organic facies are mixed with 1: 1～1: 100 volume ratio, holding temperature is at 10-200 ℃, react after 1-24 hour, tell the nano metal organic solution that organic facies just can obtain functionalization, metal nanoparticle is: Pd, Pt, Rh, Ru, Ir, Au, Ag, Co, Ni;
2. a kind of method for preparing functional metal nano particles according to claim 1, it is characterized in that, described organic facies is meant the organic solvent immiscible with water, comprises cyclohexane, n-hexane, normal heptane, normal octane, positive nonane, n-decane, benzene,toluene,xylene;
3. a kind of method for preparing functional metal nano particles according to claim 1 is characterized in that described water-soluble metal salt comprises: PdCl
2, PtCl
2, RhCl
3, RuCl
3, HAuCl
4, AgNO
3, Ag (NH
3)
2NO
3, CoNO
3, NiNO
3
4. a kind of method for preparing functional metal nano particles according to claim 1; it is characterized in that; described organic protection reagent is organic amine, organic mercaptan and organophosphor; comprise: lauryl amine, tetradecy lamine, cetylamine, octadecylamine, aromatic amine and have substituent aromatic amine; lauryl mercaptan, tetradecanylthioalcohol, 16 mercaptan, stearylmercaptan, aromatic thiol and have substituent aromatic thiol; the organic reagent that contains amido and sulfydryl simultaneously: p-Mercaptoaniline, organophosphor is as triphenyl phosphorus, triethyl phosphine.
5. a kind of method for preparing functional metal nano particles according to claim 1, it is characterized in that, described organic reducing agent is organic aldehydes and organic hydrazine class, comprising: formaldehyde, acetaldehyde, propionic aldehyde, benzaldehyde, phenylacetaldehyde, furfural, phenylhydrazine, to procarbazine.
6. a kind of method for preparing functional metal nano particles according to claim 1 is characterized in that the temperature of described preparation metal nanoparticle is 20-180 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610047260 CN1899733A (en) | 2006-07-18 | 2006-07-18 | New method for preparing functional metal nano particles |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610047260 CN1899733A (en) | 2006-07-18 | 2006-07-18 | New method for preparing functional metal nano particles |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1899733A true CN1899733A (en) | 2007-01-24 |
Family
ID=37655828
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610047260 Pending CN1899733A (en) | 2006-07-18 | 2006-07-18 | New method for preparing functional metal nano particles |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1899733A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199407A (en) * | 2011-03-18 | 2011-09-28 | 中科院广州化学有限公司 | High-dispersing nanometer silver and high-performance conductive adhesive |
| CN103056384A (en) * | 2013-01-07 | 2013-04-24 | 济南大学 | Preparation method of precious metal and magnetic nano particles |
| CN103115955A (en) * | 2013-01-21 | 2013-05-22 | 张琦 | Application of self-assembled film in surface auxiliary laser desorption or ionization flying time mass spectrum |
| CN103157808A (en) * | 2013-02-01 | 2013-06-19 | 天津商业大学 | Gold, platinum and ruthenium alloy nanometer particle and preparation method of colloid disperse system thereof |
| CN104684669A (en) * | 2012-10-01 | 2015-06-03 | 同和电子科技有限公司 | Method for producing fine silver particles |
| CN104736276A (en) * | 2012-08-23 | 2015-06-24 | 三星精密化学株式会社 | Method for manufacturing metal nanoparticles by using phase transition reduction, and metal ink comprising metal nanoparticles manufactured thereby |
| CN109420774A (en) * | 2017-08-28 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of preparation of the controllable AgAu alloy nanocluster of atom number, size |
| CN109622985A (en) * | 2018-12-11 | 2019-04-16 | 有研亿金新材料有限公司 | A kind of preparation method of high decentrality submicron grade bronze |
| CN110405224A (en) * | 2019-08-13 | 2019-11-05 | 大连理工大学 | A method of using aminothiophenol as one step rapid synthesis copper nano-cluster of ligand |
-
2006
- 2006-07-18 CN CN 200610047260 patent/CN1899733A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199407A (en) * | 2011-03-18 | 2011-09-28 | 中科院广州化学有限公司 | High-dispersing nanometer silver and high-performance conductive adhesive |
| CN104736276A (en) * | 2012-08-23 | 2015-06-24 | 三星精密化学株式会社 | Method for manufacturing metal nanoparticles by using phase transition reduction, and metal ink comprising metal nanoparticles manufactured thereby |
| CN104684669A (en) * | 2012-10-01 | 2015-06-03 | 同和电子科技有限公司 | Method for producing fine silver particles |
| CN103056384A (en) * | 2013-01-07 | 2013-04-24 | 济南大学 | Preparation method of precious metal and magnetic nano particles |
| CN103056384B (en) * | 2013-01-07 | 2015-02-18 | 济南大学 | Preparation method of precious metal and magnetic nano particles |
| CN103115955A (en) * | 2013-01-21 | 2013-05-22 | 张琦 | Application of self-assembled film in surface auxiliary laser desorption or ionization flying time mass spectrum |
| CN103157808A (en) * | 2013-02-01 | 2013-06-19 | 天津商业大学 | Gold, platinum and ruthenium alloy nanometer particle and preparation method of colloid disperse system thereof |
| CN109420774A (en) * | 2017-08-28 | 2019-03-05 | 中国科学院大连化学物理研究所 | A kind of preparation of the controllable AgAu alloy nanocluster of atom number, size |
| CN109622985A (en) * | 2018-12-11 | 2019-04-16 | 有研亿金新材料有限公司 | A kind of preparation method of high decentrality submicron grade bronze |
| CN110405224A (en) * | 2019-08-13 | 2019-11-05 | 大连理工大学 | A method of using aminothiophenol as one step rapid synthesis copper nano-cluster of ligand |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1899733A (en) | New method for preparing functional metal nano particles | |
| US7413770B2 (en) | Ethylene glycol monolayer protected nanoparticles | |
| Maity et al. | Dendrimer-encapsulated copper cluster as a chemoselective and regenerable hydrogenation catalyst | |
| KR100716201B1 (en) | Metal nanoparticles and method for manufacturing thereof | |
| CN102064311B (en) | Preparation method of carbon nanometer tube metal particle composite | |
| Lu et al. | Polymer-protected Ni/Pd bimetallic nano-clusters: preparation, characterization and catalysis for hydrogenation of nitrobenzene | |
| CN103827035B (en) | The preparation method of the amount of metal submanifold of molecule constraint form | |
| Chandler et al. | Dendrimer-encapsulated bimetallic nanoparticles: synthesis, characterization, and applications to homogeneous and heterogeneous catalysis | |
| Mayer et al. | Palladium and platinum nanocatalysts protected by amphiphilic block copolymers | |
| CN104844408B (en) | A kind of it is catalyzed the australene Hydrogenation method for cis-pinane | |
| CN101690977B (en) | Preparation method of hollow noble metal nanoparticles | |
| CN105170161B (en) | Hydrotalcite loads Au25‑xPdxCluster catalyst and preparation method thereof | |
| EP2882550B1 (en) | One pot process for the preparation of ultra-small size transition metal nanoparticles | |
| CN105543211A (en) | Immobilized glucose oxidase as well as preparation method and application thereof | |
| Noël et al. | Cyclodextrins as multitask agents for metal nano-heterogeneous catalysis: A review | |
| CN114682303A (en) | Preparation method for synthesizing noble metal @ MOF core-shell catalyst by in-situ one-step method | |
| JPH09225317A (en) | Nickel/noble metal binary metal cluster and catalyst made from the cluster and its preparation | |
| Blanckenberg et al. | Effect of nanoparticle metal composition: mono-and bimetallic gold/copper dendrimer stabilized nanoparticles as solvent-free styrene oxidation catalysts | |
| CN110327975B (en) | Hydroformylation catalyst, preparation method and application thereof | |
| Reddy et al. | Pd/chitosan nanoparticle catalysts prepared by solid mortar grinding for hydrogenation of nitroarenes | |
| JP5062506B2 (en) | Extraction method of metal fine particles | |
| Yasukawa et al. | Chiral metal nanoparticles for asymmetric catalysis | |
| KR20160119090A (en) | Process for manufacturing supported nanocolloidal particles, and supported nanocolloidal particles | |
| Crockett et al. | Impact on the Formation and Catalytic Property of Pt-Based Nanocatalysts by Galvanic Reaction with Co-Reduction Agents | |
| Toshima | Inorganic nanoparticles for catalysis |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |