CN105032413A - Quick preparation method of Au-supported carbon nano-particles with visible light - Google Patents
Quick preparation method of Au-supported carbon nano-particles with visible light Download PDFInfo
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- CN105032413A CN105032413A CN201510015339.3A CN201510015339A CN105032413A CN 105032413 A CN105032413 A CN 105032413A CN 201510015339 A CN201510015339 A CN 201510015339A CN 105032413 A CN105032413 A CN 105032413A
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Abstract
The invention discloses a quick preparation method of Au-supported carbon nano-particles with visible light, which comprises the following steps: (A) placing graphite into a three-mouth flask filled with H5PMo10V2O40, assembling a reflux apparatus and stirring the reactants, and performing reflux under a boiled status at 140 DEG C for 24 h; (B) cooling the three-mouth flask to normal temperature, feeding the reflux liquid into a dialytic bag, and performing osmosis to the dialytic bag in deionized water; (C) after osmosis, regulating the pH value of the solution in the dialytic bag to 6.5; (D) moving the solution to a centrifugal tube and performing centrifugation, and diluting 5 ml of a supernatant liquor to 50 ml; (E) introducing the diluted solution into a photo-reactor and irradiating the photo-reactor, and meanwhile adding 0.5 ml of a 0.1 M HAuCl4.3H2O solution quickly in several times into the reactor to obtain a suspension liquid after the reaction is finished; and (F) drying the suspension liquid to obtain the solid Au-supported carbon nano-particles. The preparation method is more economical, convenient and environment-friendly.
Description
Technical field
The present invention relates to the preparation method of nano-sized carbon, especially relate to the preparation method of the carbon nano-particle of a kind of load Au.
Background technology
Different carbon nanomaterials has different functions, and as graphitic carbon nano particle has powerful adsorption capacity, easy and histocyte adsorbs.This type nano granular has good cell compatibility, enhancement effect, has very large potential value in cytology field.As brand-new material, carbon nanomaterial also plays an important role in military project national defence; The surface-functionalized carbon nano-particle with gold or platinum coating can be used as photo-reduction agent catalysis CO
2be converted into hydrocarbon; Fluorescent carbon nano particle not only has good biocompatibility and is easy to the advantage such as surface-functionalized, also has can realize conversion fluorescence and launch and the characteristic of stable luminescence, so have important using value at biomedicine field.Carbon nanomaterial is varied, has different features and application separately.
At present, the preparation method of carbon nano-particle can be divided into two classes: method and from bottom to top method from top to bottom.Namely method peels off the physical method preparing carbon nano-particle from larger carbon structure from top to bottom, mainly comprises: arc discharge method, laser ablation method, electrochemical process, acid return cooking method.Namely method is prepared the chemical method of carbon nano-particle by molecular precursor from bottom to top, mainly comprises: support synthetic method, organic carbon method.There is certain deficiency in these synthetic methods, the pattern of carbon nano-particle, output and difficult quality reach accurate control separately, and the time of preparing finished product, at least more than 5 days, can not reach large-scale simple synthesis.Also discussion is lacked for its growth mechanism, particularly because the restriction of synthetic method makes it still be in the starting stage in the research of application aspect.
Summary of the invention
The present invention, in order to overcome above-mentioned deficiency, provides the fast preparation method of the carbon nano-particle of a kind of visible ray load Au, more economic, the convenient and environmental protection when preparing the carbon nano-particle of load Au.
Technical scheme of the present invention is as follows:
A preparation method for the carbon nano-particle of load Au, comprises the following steps:
(1) get graphite to put into H is housed
5pMo
10v
2o
40there-necked flask in, put up reflux, and at room temperature stir 30min, then reflux 2h under 140 DEG C of fluidized states;
(2) there-necked flask is cooled to normal temperature, phegma is imported in bag filter, then this bag filter is permeated in deionized water;
(3) after infiltration, by the solution adjust ph in bag filter to 6.5;
(4) above-mentioned solution being loaded centrifuge tube carries out centrifugal;
(5) centrifugal complete after, get supernatant liquor 5ml, be diluted to 50ml by deionized water;
(6) step (5) is diluted in the solution lead-in light reactor obtained and irradiate;
(7) HAuCl of 0.5ml, 0.1M is prepared
43H
2o solution, divides and joins in above-mentioned reactor by this solution 5 times;
(8) reaction obtains suspension after terminating, and is dried by suspension, obtains the carbon nano-particle of solid particle load Au.
Wherein, step has got 1g graphite in (1), and the H of 5M, 150ml is housed in there-necked flask
5pMo
10v
2o
40.
Time of penetration in step (2) is 1 day, and every 6 hours need change water once.
The ammoniacal liquor of 0.25M is used to regulate pH in step (3).
With the centrifugation 1h of 1500r/min in step (4).
Light source in step (6) is high performance analog daylight xenon light source, and irradiation time is 60 minutes.
By HAuCl in step (7)
43H
2the O solution time interval joined in reactor is 5min.
Bake out temperature in step (8) is 40 DEG C, and drying time is 2h.
The invention has the beneficial effects as follows:
The advantages such as the present invention has can continuous seepage, low in the pollution of the environment, more economic, the convenient and environmental protection when preparing the carbon nano-particle of load Au.
Accompanying drawing explanation
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein:
Fig. 1 is that the carbon nano-particle UV of load Au schemes;
Fig. 2 is the carbon nano-particle particle diameter resolution chart of load Au;
Fig. 3 is the SEM figure of raw graphite;
Fig. 4 is that the carbon nano-particle TEM of load Au schemes.
Detailed description of the invention
Arbitrary feature disclosed in this description, unless specifically stated otherwise, all can be replaced by other equivalences or the alternative features with similar object.That is, unless specifically stated otherwise, each feature is an example in a series of equivalence or similar characteristics.
A fast preparation method for the carbon nano-particle of visible ray load Au, preparation method is as follows: get 1g graphite, put into and 5M, 150mlH are housed
5pMo
10v
2o
40there-necked flask in, put up reflux.Stirred at ambient temperature 30min, then under 140 DEG C of fluidized states, backflow 2h.Treat that there-necked flask is cooled to normal temperature, imported by phegma in the bag filter of 500 models, this bag filter permeates 1 day in deionized water, and every 6 hours of period changed water once.After infiltration, by the solution in bag filter by 0.25M ammoniacal liquor adjust ph to 6.5.Above-mentioned solution is loaded centrifuge tube, centrifugal 1 hour of 1500r/min.Centrifugal complete after, get supernatant liquor 5ml, be diluted to 50ml by deionized water.Imported by above-mentioned solution in homemade Photoreactor, light source is high performance analog daylight xenon light source, irradiates 60 minutes.Prepare 0.5ml0.1MHAuCl simultaneously
43H
2o solution, added this solution 0.1ml in above-mentioned reactor, adds 5 these solution altogether every 5 minutes.Obtain suspension after reaction terminates, suspension is dried 2h at 40 DEG C, and the solid particle obtained after oven dry is the carbon nano-particle of load Au.
Solid particle samples obtained above is carried out the analysis (see Fig. 1) of ultraviolet sign by ultraviolet-uisible spectrophotometer (UV) (T6 Beijing Pu Xi all purpose instrument Co., Ltd), wavelength is 210-800nm.
As shown in Figure 1, there is the characteristic peak of obvious Au at 537nm place.In figure, curve a is the carbon nano-particle curve before load Au, from this curve, is carbon particle curve; Curve f is that HAuCl43H2O original solution UV schemes; Curve b is that load Au60minUV schemes, curve c is that 180minUV schemes, curve d is that 240minUV schemes, curve e is 360minUV figure.Known load time 60min just has Au to separate out.Further demonstrate that product is exactly the carbon nano-particle of load Au.
Solid particle samples obtained above is undertaken analyzing (see Fig. 2) by nano-particle size analysis instrument (NANOPHOXParticleSizeAnalysis), test specification: 1-10000nm, concentration range: ppm-70vol.%, light source: He-Ne Lasers, wavelength 632.8nm, laser power: 10mw, temperature: 15-40 DEG C, humidity 20-70% frozen-free.
As shown in Figure 2, the carbon nano-particle particle diameter of load Au is about 1.2nm, can obtain thus, has successfully prepared the carbon nano-particle of load Au.
As shown in Figure 3 and Figure 4, Fig. 4 is the TEM figure testing the solid particle obtained, Au particulate load on carbon particles as seen from Figure 4, Fig. 3 is the SEM figure of graphite, and graphite presents sheet, the granular carbon nano-particle of dense distribution in figure, particle diameter is between 1-1.5nm, compared with Fig. 3, can know that the lamellar structure of graphite is destroyed, nano level carbon granule is prepared.
The present invention is not limited to aforesaid detailed description of the invention.The present invention expands to any new feature of disclosing in this manual or any combination newly, and the step of the arbitrary new method disclosed or process or any combination newly.
Claims (8)
1. a preparation method for the carbon nano-particle of load Au, is characterized in that, comprises the following steps:
(1) get graphite to put into H is housed
5pMo
10v
2o
40there-necked flask in, put up reflux, and at room temperature stir 30min, then reflux 2h under 140 DEG C of fluidized states;
(2) there-necked flask is cooled to normal temperature, phegma is imported in bag filter, then this bag filter is permeated in deionized water;
(3) after infiltration, by the solution adjust ph in bag filter to 6.5;
(4) above-mentioned solution being loaded centrifuge tube carries out centrifugal;
(5) centrifugal complete after, get supernatant liquor 5ml, be diluted to 50ml by deionized water;
(6) step (5) is diluted in the solution lead-in light reactor obtained and irradiate;
(7) HAuCl of 0.5ml, 0.1M is prepared
43H
2o solution, divides and joins in above-mentioned reactor by this solution 5 times;
(8) reaction obtains suspension after terminating, and is dried by suspension, obtains the nano carbon particle of solid particle load Au.
2. the preparation method of the nano carbon particle of load Au according to claim 1, is characterized in that, step has got 1g graphite in (1), and the H of 5M, 150ml is housed in there-necked flask
5pMo
10v
2o
40.
3. the preparation method of the nano carbon particle of load Au according to claim 1, is characterized in that, the time of penetration in step (2) is 1 day.
4. the preparation method of the nano carbon particle of load Au according to claim 1, is characterized in that, uses the ammoniacal liquor of 0.25M to regulate pH in step (3).
5. the preparation method of the nano carbon particle of load Au according to claim 1, is characterized in that, with the centrifugation 1h of 1500r/min in step (4).
6. the fast preparation method of the carbon nano-particle of visible ray load Au according to claim 1, is characterized in that, the light source in step (6) is high performance analog daylight xenon light source, and irradiation time is 60 minutes.
7. the preparation method of the nano carbon particle of load Au according to claim 1, is characterized in that, by HAuCl in step (7)
43H
2the O solution time interval joined in reactor is 5min.
8. the preparation method of the nano carbon particle of load Au according to claim 1, is characterized in that, the bake out temperature in step (8) is 40 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105797772A (en) * | 2016-04-25 | 2016-07-27 | 宁波工程学院 | Doped heteropolyacid catalyst and method for producing hydrogen by photolyzing water under visible light |
| CN105833908A (en) * | 2016-04-26 | 2016-08-10 | 宁波工程学院 | Doped heteropolyacid catalyst and method for photolyzing water to generate hydrogen under visible light |
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| CN103084175A (en) * | 2013-01-31 | 2013-05-08 | 武汉大学 | Pt-Au@Pt core-shell structure fuel cell cathode catalyst and preparation method thereof |
| CN103165914A (en) * | 2011-12-15 | 2013-06-19 | 中国科学院大连化学物理研究所 | Pt/Au/PdCo/C catalyst, and preparation and application thereof |
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Patent Citations (5)
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| US20120058888A1 (en) * | 2004-10-29 | 2012-03-08 | Umicore Ag & Co. Kg | Method for manufacture of noble metal alloy catalysts and catalysts prepared therewith |
| CN103165914A (en) * | 2011-12-15 | 2013-06-19 | 中国科学院大连化学物理研究所 | Pt/Au/PdCo/C catalyst, and preparation and application thereof |
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| CN105797772A (en) * | 2016-04-25 | 2016-07-27 | 宁波工程学院 | Doped heteropolyacid catalyst and method for producing hydrogen by photolyzing water under visible light |
| CN105797772B (en) * | 2016-04-25 | 2018-06-05 | 宁波工程学院 | A kind of doping heteropolyacid catalyst and the under visible light method of photolysis water hydrogen gas |
| CN105833908A (en) * | 2016-04-26 | 2016-08-10 | 宁波工程学院 | Doped heteropolyacid catalyst and method for photolyzing water to generate hydrogen under visible light |
| CN105833908B (en) * | 2016-04-26 | 2018-06-01 | 宁波工程学院 | A kind of doping heteropolyacid catalyst and the under visible light method of photolysis water hydrogen gas |
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