CN101444730A - Method for preparing carbon nano-fiber/silver nano-particle composite catalyst - Google Patents
Method for preparing carbon nano-fiber/silver nano-particle composite catalyst Download PDFInfo
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- CN101444730A CN101444730A CNA2007101874563A CN200710187456A CN101444730A CN 101444730 A CN101444730 A CN 101444730A CN A2007101874563 A CNA2007101874563 A CN A2007101874563A CN 200710187456 A CN200710187456 A CN 200710187456A CN 101444730 A CN101444730 A CN 101444730A
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Abstract
The invention discloses a method for preparing carbon nano-fiber/silver nano-particle composite catalyst; the method uses DMSO as a reducer to reduce silver nitrate so as to gain silver nano-particle and load the silver nano-particle onto the surface of the carbon nano-fiber. The silver nano-particle prepared by the method has small particle size and can be uniformly dispersed on the surface of the carbon nano-fiber. The method has simple preparation method and process, moderate condition, low preparation cost and can gain the carbon nano-fiber/silver nano-particle composite catalyst with small particle size and high dispersibility.
Description
Technical field:
The present invention relates to a kind of preparation method of carbon nano-fiber/silver nano-particle composite catalyst
Background technology:
Carbon nano-fiber is meant fibre diameter＜100nm, and fibre length is at several microns, the nano-carbon material with bigger draw ratio.Carbon nano-fiber is owing to its outstanding physics, chemical property have obtained using widely as the basic material of science and technology field, especially the special porous surface structure of carbon nano-fiber makes carbon nano-fiber have big specific area, becomes the preferred material of catalyst carrier.Up to the present, carbon nano-fiber has been used for preparing various composites, comprise polymer/carbon nano-fiber composite, metal/nanometer carbon fibre composite or the like, wherein with metal (Au, Pt, Ag) or binary alloy nanoparticle/carbon nano-fiber compound catalyze material comparatively more sees, mainly be the electrode catalyst that is used for doing the electrochemical reaction of fuel cell.At present, bibliographical information is more is with the act as a fuel electrode catalytic materials of battery of platinum/material with carbon element, but because costing an arm and a leg of metal platinum makes its application be subjected to certain restriction.Yet, if just can reduce application cost with the alternative nano platinum particle of the silver of nano-scale, but the problem that the pertinent literature of silver/carbon catalysis material exists mainly is dispersed poor at carbon material surface of big (20-40nm) and Nano silver grain of Nano silver grain size ratio, and agglomeration is obvious.With this method can prepare Nano silver grain particle diameter little (approximately 5nm) and can homogeneous be distributed to the carbon nano-fiber surface, the composite for preparing can be used as the electrochemical catalysis material, is applied in the ion-exchange membrane electrolyzer gas-diffusion electrode Catalytic Layer.So the carbon nano-fiber that innovative point of the present invention just is to have selected high-ratio surface for use helps the dispersion of metallic catalyst at carrier surface as catalyst carrier; Prepared of the electrochemical catalysis material agent of the little silver-colored high degree of dispersion of nano-scale, remedied the weak point of pertinent literature at carrier surface.
Summary of the invention:
The present invention is directed to the problems referred to above, propose the method for the Nano silver grain/carbon nano-fiber composite of a kind of easy preparation small particle diameter and polymolecularity, and use cheap chemical reagent, preparation cost is low.
Technical scheme provided by the invention is: be source metal with the silver nitrate, dimethyl sulfoxide (DMSO) (DMSO) is as reducing agent, natrium citricum (Na
3CitH
2O) as stabilizing agent, the acid-treated carbon nano-fiber of process is as carrier.Adopt the method for electronation, prepare the Nano silver grain colloid earlier, be mixed with out the little Nano silver grain of particle diameter with ultrasonic finely dispersed carbon nano-fiber dispersion at 60 ℃ then and be dispersed in the carbon nano-fiber surface equably, obtained Nano silver grain/carbon nano-fiber composite.
Advantage of the present invention: preparation method and process are simple, mild condition, and preparation cost is low and can to obtain particle diameter little and have a silver/carbon nano-fiber composite of polymolecularity.
Description of drawings:
Fig. 1 is preparation flow figure of the present invention
The X-ray diffraction analysis figure of the composite that Fig. 2 prepares for the present invention
The electron scanning micrograph of the composite that Fig. 3 prepares for the present invention
The efficient projection electron microscope photo of the composite that Fig. 4 prepares for the present invention.
The specific embodiment:
Referring to Fig. 1, at first dimethyl sulfoxide (DMSO) is warmed up to 60 ℃ silver nitrate aqueous solution joined in the dimethyl sulfoxide (DMSO), subsequently natrium citricum is joined above-mentioned reaction system and prepare the Nano silver grain colloid.In preparation Nano silver grain colloid,, obtain the decentralized photo of homogeneous the ultrasonic dispersion in dimethyl sulfoxide (DMSO) (DMSO) of the carbon nano-fiber after the acid treatment.At last, with the homogeneous decentralized photo mixing of Nano silver grain colloid and carbon nano-fiber, stir and obtain product.
The carbon nano-fiber of getting after the 0.05g acid treatment joins in the 30ml dimethyl sulfoxide (DMSO) (DMSO), and ultrasonic wave disperses 30min; Get in the dimethyl sulfoxide (DMSO) (30ml) that silver nitrate 1.4ml (0.1mol/L) joins 60 ℃ of 30ml and follow magnetic agitation, add natrium citricum (Na afterwards
3CitH
2O) 2.8ml (0.1mol/L) stirs 30min, obtains the Nano silver grain colloid.At last the Nano silver grain colloid for preparing is mixed at 60 ℃ with the carbon nano-fiber decentralized photo and continue to stir 20min, with the reaction system filtration under diminished pressure that obtains and use the washed with de-ionized water multipass, 80 ℃ of dryings can obtain Nano silver grain/carbon nano-fiber composite in 24 hours in vacuum drying chamber.
The consumption that changes silver nitrate can change the load capacity (10wt%-30wt%) of Nano silver grain on the carbon nano-fiber surface.
Claims (8)
1, a kind of chemical reduction method prepares the method for carbon nano-fiber/silver nano-particle composite catalyst, it is characterized in that: prepare the Nano silver grain colloid with chemical reduction method earlier, then this Nano silver grain colloid is mixed with the decentralized photo of carbon nano-fiber, thereby the Nano silver grain of polymolecularity is loaded to the carbon nano-fiber surface.
2, preparation method according to claim 1 is characterized in that: will handle through nitration mixture as the carrier and the carbon nano-fiber of Nano silver grain with carbon nano-fiber: sulfuric acid/nitric acid, and volume ratio=3:1,60 ℃ were refluxed 5 hours.
3, preparation method according to claim 1 is characterized in that: make solvent and reducing agent prepares the Nano silver grain colloid with dimethyl sulfoxide (DMSO) (DMSO).
4, preparation method according to claim 1 is characterized in that: with natrium citricum (Na
3CitH
2O) as catcher, the stabilizing agent of Nano silver grain.
5, preparation method according to claim 1 is characterized in that: natrium citricum (Na
3CitH
2O) concentration range is controlled at 10
-3Mol/L to 1mol/L.
6, preparation method according to claim 1 is characterized in that: silver nitrate (AgNO
3) concentration range is controlled at 10
-3Mol/L to 1mol/L.
7, preparation method according to claim 1 is characterized in that: the concentration of stabilizing agent natrium citricum is consistent with the concentration of silver nitrate.
8, preparation method according to claim 1 is characterized in that: temperature in Nano silver grain colloid and the process that the carbon nano-fiber decentralized photo mixes should be controlled at 60 ℃, and stir 20min to 2h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710187456 CN101444730B (en) | 2007-11-27 | 2007-11-27 | Method for preparing carbon nano-fiber/silver nano-particle composite catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710187456 CN101444730B (en) | 2007-11-27 | 2007-11-27 | Method for preparing carbon nano-fiber/silver nano-particle composite catalyst |
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| CN101444730A true CN101444730A (en) | 2009-06-03 |
| CN101444730B CN101444730B (en) | 2011-07-27 |
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| CN 200710187456 Expired - Fee Related CN101444730B (en) | 2007-11-27 | 2007-11-27 | Method for preparing carbon nano-fiber/silver nano-particle composite catalyst |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016007113A1 (en) * | 2014-07-08 | 2016-01-14 | Tovaristvo Z Obmezhenou Vidpovidalnistu "Nanomedtrast" | Biocompatible colloidal solution of silver nanoparticles in non-aqueous polar solvent and method of obtaining thereof |
| CN106179335A (en) * | 2016-07-05 | 2016-12-07 | 张启辉 | The preparation method of carbon silver composite catalyst |
| CN107812520A (en) * | 2017-11-08 | 2018-03-20 | 扬州大学 | A kind of loading type silver catalyst preparation method for purifying formaldehyde |
| CN108619791A (en) * | 2018-05-05 | 2018-10-09 | 安徽乐金环境科技有限公司 | A kind of purifying formaldehyde strainer |
| CN108620039A (en) * | 2018-05-05 | 2018-10-09 | 安徽乐金环境科技有限公司 | Activate the preparation method of Compound adsorption type purifying indoor formaldehyde agent |
| CN108620067A (en) * | 2018-05-05 | 2018-10-09 | 安徽乐金环境科技有限公司 | A kind of preparation method of silver-based formaldehyde absorbing catalyst |
| CN108654570A (en) * | 2018-05-05 | 2018-10-16 | 安徽乐金环境科技有限公司 | Activate Compound adsorption type purifying indoor formaldehyde agent |
| CN108654210A (en) * | 2018-05-05 | 2018-10-16 | 安徽乐金环境科技有限公司 | A kind of activation Compound adsorption type purifying indoor formaldehyde strainer and preparation method thereof |
| CN108816222A (en) * | 2018-05-05 | 2018-11-16 | 安徽乐金环境科技有限公司 | A kind of silver-based formaldehyde absorbing catalyst |
| CN113119256A (en) * | 2021-04-16 | 2021-07-16 | 北京林业大学 | Preparation method of conductive wood aerogel |
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| CN1094404C (en) * | 1999-10-20 | 2002-11-20 | 中山大学 | Method for making nanometer noble metal microparticles |
| CN1424149A (en) * | 2002-12-27 | 2003-06-18 | 浙江大学 | Method for coating mono-metal particles on carbon nano tube surface |
| JP2003295387A (en) * | 2002-03-29 | 2003-10-15 | Konica Corp | Heat-developable material |
| CN1493711A (en) * | 2002-11-01 | 2004-05-05 | 中国科学院理化技术研究所 | Preparation method of carbon nano tube/silver composite functional material |
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2007
- 2007-11-27 CN CN 200710187456 patent/CN101444730B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1094404C (en) * | 1999-10-20 | 2002-11-20 | 中山大学 | Method for making nanometer noble metal microparticles |
| JP2003295387A (en) * | 2002-03-29 | 2003-10-15 | Konica Corp | Heat-developable material |
| CN1493711A (en) * | 2002-11-01 | 2004-05-05 | 中国科学院理化技术研究所 | Preparation method of carbon nano tube/silver composite functional material |
| CN1424149A (en) * | 2002-12-27 | 2003-06-18 | 浙江大学 | Method for coating mono-metal particles on carbon nano tube surface |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016007113A1 (en) * | 2014-07-08 | 2016-01-14 | Tovaristvo Z Obmezhenou Vidpovidalnistu "Nanomedtrast" | Biocompatible colloidal solution of silver nanoparticles in non-aqueous polar solvent and method of obtaining thereof |
| CN106179335A (en) * | 2016-07-05 | 2016-12-07 | 张启辉 | The preparation method of carbon silver composite catalyst |
| CN107812520A (en) * | 2017-11-08 | 2018-03-20 | 扬州大学 | A kind of loading type silver catalyst preparation method for purifying formaldehyde |
| CN108619791A (en) * | 2018-05-05 | 2018-10-09 | 安徽乐金环境科技有限公司 | A kind of purifying formaldehyde strainer |
| CN108620039A (en) * | 2018-05-05 | 2018-10-09 | 安徽乐金环境科技有限公司 | Activate the preparation method of Compound adsorption type purifying indoor formaldehyde agent |
| CN108620067A (en) * | 2018-05-05 | 2018-10-09 | 安徽乐金环境科技有限公司 | A kind of preparation method of silver-based formaldehyde absorbing catalyst |
| CN108654570A (en) * | 2018-05-05 | 2018-10-16 | 安徽乐金环境科技有限公司 | Activate Compound adsorption type purifying indoor formaldehyde agent |
| CN108654210A (en) * | 2018-05-05 | 2018-10-16 | 安徽乐金环境科技有限公司 | A kind of activation Compound adsorption type purifying indoor formaldehyde strainer and preparation method thereof |
| CN108816222A (en) * | 2018-05-05 | 2018-11-16 | 安徽乐金环境科技有限公司 | A kind of silver-based formaldehyde absorbing catalyst |
| CN113119256A (en) * | 2021-04-16 | 2021-07-16 | 北京林业大学 | Preparation method of conductive wood aerogel |
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| Publication number | Publication date |
|---|---|
| CN101444730B (en) | 2011-07-27 |
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