CN105032413B - The fast preparation method of the carbon nano-particle of visible ray load Au - Google Patents
The fast preparation method of the carbon nano-particle of visible ray load Au Download PDFInfo
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- CN105032413B CN105032413B CN201510015339.3A CN201510015339A CN105032413B CN 105032413 B CN105032413 B CN 105032413B CN 201510015339 A CN201510015339 A CN 201510015339A CN 105032413 B CN105032413 B CN 105032413B
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Abstract
The invention discloses a kind of fast preparation method of the carbon nano-particle of visible ray load Au, comprise the following steps：Graphite is taken to put into equipped with H5PMo10V2O40There-necked flask in, put up reflux, and stir, then flow back 24h under 140 DEG C of fluidized states；There-necked flask is cooled to normal temperature, phegma is imported in bag filter, then the bag filter is permeated in deionized water；The solution in bag filter is adjusted into pH value to 6.5 after infiltration；Above-mentioned solution loading centrifuge tube is centrifuged, supernatant liquor 5ml is taken afterwards, 50ml is diluted to deionized water；The solution for obtaining will be diluted and imported in Photoreactor and irradiated, the HAuCl of 0.5ml, 0.1M that period will prepare simultaneously4·3H2O solution is quickly added in reactor several times；Reaction obtains suspension after terminating, and suspension is dried, and obtains the nano carbon particle that solid particle loads Au.More economic, convenient and environmental protection of the invention.
Description
Technical field
The present invention relates to the preparation method of nano-sized carbon, more particularly, to a kind of preparation side of the carbon nano-particle of load Au
Method.
Background technology
Different carbon nanomaterials has different functions, and such as graphitic carbon nano particle has powerful adsorption capacity, holds
Easily adsorbed with histocyte.The type nano granular has good cell compatibility, enhancement effect, has very big in cytology field
Potential value.Used as brand-new material, carbon nanomaterial also plays an important role in terms of military project national defence；With golden or platinum coating
Surface-functionalized carbon nano-particle can be catalyzed CO as photo-reduction agent2It is converted into hydrocarbon；Fluorescence carbon nano-particle is not only
There is good biocompatibility and be easy to surface-functionalized, also launch with achievable conversion fluorescence and luminous steady
Fixed characteristic, so having important application value in biomedicine field.Carbon nanomaterial is varied, each with different
Feature and application.
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.From top to bottom
Method is the physical method that carbon nano-particle is prepared from larger carbon structure peeling, is mainly included：Arc discharge method, laser ablation
Cooking method is returned in method, electrochemical process, acid.Method is the chemical method that carbon nano-particle is prepared by molecular precursor from bottom to top, main bag
Include：Support synthetic method, organic carbon method.These synthetic methods are individually present certain deficiency, the pattern of carbon nano-particle, product
Amount and quality are difficult to reach precise control, prepare the time of finished product at least more than 5 days, it is impossible to reach large-scale simple
Synthesis.Also lack discussion for its growth mechanism, especially because the limitation of synthetic method make its application aspect research still
In the starting stage.
The content of the invention
The present invention is above-mentioned in order to overcome the shortcomings of, there is provided a kind of quick preparation of the carbon nano-particle of visible ray load Au
Method, more economic, the convenient and environmental protection when the carbon nano-particle of load Au is prepared.
Technical scheme is as follows：
A kind of preparation method of the carbon nano-particle of load Au, comprises the following steps：
(1) graphite is taken to put into equipped with H5PMo10V2O40There-necked flask in, put up reflux, and be stirred at room temperature
30min, then flow back 2h under 140 DEG C of fluidized states；
(2) there-necked flask is cooled to normal temperature, phegma is imported in bag filter, then by the bag filter in deionized water
Infiltration；
(3) after permeating, the solution in bag filter is adjusted into pH value to 6.5；
(4) above-mentioned solution loading centrifuge tube is centrifuged；
(5) after the completion of being centrifuged, supernatant liquor 5ml is taken, 50ml is diluted to deionized water；
(6) solution that step (5) dilution is obtained is imported in Photoreactor and is irradiated；
(7) HAuCl of 0.5ml, 0.1M is prepared4·3H2O solution, divides 5 times and the solution is added in above-mentioned reactor；
(8) reaction obtains suspension after terminating, and suspension is dried, and obtains the carbon nano-particle that solid particle loads Au.
Wherein, 1g graphite has been taken in step (1), the H equipped with 5M, 150ml in there-necked flask5PMo10V2O40。
Time of penetration in step (2) is 1 day, and need to change water once in every 6 hours.
In step (3) pH is adjusted using the ammoniacal liquor of 0.25M.
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)4·3H2The time interval that O solution is added in reactor is 5min.
Drying temperature in step (8) is 40 DEG C, and drying time is 2h.
The beneficial effects of the invention are as follows：
The present invention has can continuously be produced, the advantages of low in the pollution of the environment, when the carbon nano-particle of load Au is prepared more
Economic, convenient and environmental protection.
Brief description of the drawings
Examples of the present invention will be described by way of reference to the accompanying drawings, wherein：
Fig. 1 is the carbon nano-particle UV figures for loading Au；
Fig. 2 is the carbon nano-particle particle diameter test chart for loading Au；
Fig. 3 is the SEM figures of raw graphite；
Fig. 4 is the carbon nano-particle TEM figures for loading Au.
Specific embodiment
Any feature disclosed in this specification, unless specifically stated otherwise, can be equivalent or with similar purpose by other
Alternative features are replaced.I.e., unless specifically stated otherwise, each feature is an example in a series of equivalent or similar characteristics
.
A kind of fast preparation method of the carbon nano-particle of visible ray load Au, preparation method is as follows：1g graphite is taken, is put into
To equipped with 5M, 150ml H5PMo10V2O40There-necked flask in, put up reflux.30min is stirred at room temperature, then 140
Under DEG C fluidized state, flow back 2h.Treat that there-necked flask is cooled to normal temperature, phegma is imported in the bag filter of 500 models, the dialysis
Bag permeates 1 day in deionized water, and every 6 hours of period changed water once.After infiltration, by the 0.25M ammoniacal liquor of the solution in bag filter
Adjust pH value to 6.5.Above-mentioned solution is loaded into centrifuge tube, 1500r/min is centrifuged 1 hour.After the completion of centrifugation, supernatant liquor is taken
5ml, 50ml is diluted to deionized water.Above-mentioned solution is imported in homemade Photoreactor, light source is high performance analog daylight
Xenon light source, irradiates 60 minutes.0.5ml 0.1M HAuCl are prepared simultaneously4·3H2O solution, the solution was added every 5 minutes
0.1ml adds 5 solution altogether in above-mentioned reactor.Reaction obtains suspension after terminating, and suspension is dried at 40 DEG C
2h, the solid particle obtained after drying is the carbon nano-particle for loading Au.
Solid particle samples obtained above are passed through into ultraviolet-uisible spectrophotometer (UV) (the general analysis all purpose instrument in T6 Beijing
Co., Ltd) analysis (see Fig. 1) of ultraviolet sign is carried out, wavelength is 210-800nm.
As shown in figure 1, occurring in that the characteristic peak of obvious Au at 537nm.In figure, curve a is that the carbon loaded before Au is received
Rice grain curve, is carbon particle curve knowable to the curve；Curve f is HAuCl43H2O original solutions UV figures；Curve b is negative
Load Au60minUV figures, curve c are that 180minUV schemes, curve d is that 240minUV schemes, curve e is that 360minUV schemes.Understand load
Time 60min just has Au to separate out.Further demonstrate that product is exactly the carbon nano-particle for loading Au.
Solid particle samples obtained above are passed through into nano-particle size analysis instrument (NANOPHOX Particle Size
Analysis (see Fig. 2), test scope) are analyzed：1-10000nm, concentration range：Ppm-70vol.%, light source：He-Ne swashs
Light, wavelength 632.8nm, laser power：10mw, temperature：15-40 DEG C, humidity 20-70% frozen-frees.
As shown in Fig. 2 the carbon nano-particle particle diameter of load Au is about 1.2nm, it can thus be concluded that, it is successfully prepared load Au's
Carbon nano-particle.
As shown in Figure 3 and Figure 4, Fig. 4 is the TEM figures of the solid particle that experiment is obtained, as seen from Figure 4 Au particulate loads
On carbon particles, Fig. 3 is the SEM figures of graphite, and graphite is presented sheet, the granular carbon nano-particle of dense distribution, grain in figure
Between 1-1.5nm, compared with Fig. 3, it is known that the lamellar structure of graphite has been destroyed, nano level carbon particle is in footpath
Through preparing.
The invention is not limited in foregoing specific embodiment.The present invention is expanded to and any in this manual disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (8)
1. a kind of preparation method of the carbon nano-particle of load Au, it is characterised in that comprise the following steps：
(1) graphite is taken to put into equipped with H5PMo10V2O40There-necked flask in, put up reflux, and be stirred at room temperature
30min, then flow back 2h under 140 DEG C of fluidized states；
(2) there-necked flask is cooled to normal temperature, phegma is imported in bag filter, then the bag filter is oozed in deionized water
Thoroughly；
(3) after permeating, the solution in bag filter is adjusted into pH value to 6.5；
(4) above-mentioned solution loading centrifuge tube is centrifuged；
(5) after the completion of being centrifuged, supernatant liquor 5mL is taken, 50mL is diluted to deionized water；
(6) solution that step (5) dilution is obtained is imported in Photoreactor and is irradiated；
(7) HAuCl of 0.5mL, 0.1M is prepared4·3H2O solution, divides 5 times and the solution is added in above-mentioned reactor；
(8) reaction obtains suspension after terminating, and suspension is dried, and obtains the nano carbon particle that solid particle loads Au.
2. the preparation method of the carbon nano-particle of load Au according to claim 1, it is characterised in that step takes in (1)
1g graphite, the H equipped with 5M, 150mL in there-necked flask5PMo10V2O40。
3. the preparation method of the carbon nano-particle of load Au according to claim 1, it is characterised in that in step (2)
Time of penetration is 1 day.
4. the preparation method of the carbon nano-particle of load Au according to claim 1, it is characterised in that step makes in (3)
PH is adjusted with the ammoniacal liquor of 0.25M.
5. the preparation method of the carbon nano-particle of load Au according to claim 1, it is characterised in that in step (4) with
The centrifugation 1h of 1500r/min.
6. the preparation method of the carbon nano-particle of load Au according to claim 1, it is characterised in that in step (6)
Light source is high performance analog daylight xenon light source, and irradiation time is 60 minutes.
7. the preparation method of the carbon nano-particle of load Au according to claim 1, it is characterised in that will in step (7)
HAuCl4·3H2The time interval that O solution is added in reactor is 5min.
8. the preparation method of the carbon nano-particle of load Au according to claim 1, it is characterised in that in step (8)
Drying temperature is 40 DEG C.
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| 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102698807A (en) * | 2012-07-03 | 2012-10-03 | 昆明理工大学 | Noble metal nano catalyst prepared from organic azo dyes functionalized carbon nano materials and preparation method of catalyst |
| CN102989450A (en) * | 2012-12-03 | 2013-03-27 | 中国科学院大连化学物理研究所 | Preparation method, structural feature and application of carrying type nanometer electrocatalyst |
| 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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| US7713910B2 (en) * | 2004-10-29 | 2010-05-11 | Umicore Ag & Co Kg | Method for manufacture of noble metal alloy catalysts and catalysts prepared therewith |
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| 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 |
| CN102698807A (en) * | 2012-07-03 | 2012-10-03 | 昆明理工大学 | Noble metal nano catalyst prepared from organic azo dyes functionalized carbon nano materials and preparation method of catalyst |
| CN102989450A (en) * | 2012-12-03 | 2013-03-27 | 中国科学院大连化学物理研究所 | Preparation method, structural feature and application of carrying type nanometer electrocatalyst |
| 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 |
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