CN105014093B - The preparation method of the carbon nano-particle of visible ray supporting Pt - Google Patents
The preparation method of the carbon nano-particle of visible ray supporting Pt Download PDFInfo
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- CN105014093B CN105014093B CN201510025624.3A CN201510025624A CN105014093B CN 105014093 B CN105014093 B CN 105014093B CN 201510025624 A CN201510025624 A CN 201510025624A CN 105014093 B CN105014093 B CN 105014093B
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Abstract
The invention discloses a kind of preparation method of the carbon nano-particle of visible ray supporting Pt, comprise the following steps：Graphite is taken to be put into equipped with H3PW12O40Three-necked flask in, put up reflux, and stir, then flow back 10h under 140 DEG C of fluidized states；Three-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 5.5 after infiltration；Above-mentioned solution loading centrifuge tube is centrifuged, supernatant liquor 5ml is taken afterwards, 50ml is diluted to deionized water；The solution that dilution is obtained, which is imported in Photoreactor, to be irradiated, during which simultaneously by 0.5ml, 0.1M of preparation H2PtCl6·6H2O solution is added in reactor several times, and regulation pH value is 5.0 6.0；Reaction obtains suspension after terminating, and suspension is dried, and obtains the carbon nano-particle that solid particle is supporting Pt.
Description
Technical field
The present invention relates to the preparation method of nano-sized carbon, more particularly, to a kind of system of the carbon nano-particle of visible ray supporting Pt
Preparation 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.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 there is 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
Method, electrochemical process, acid return cooking method.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.Certain deficiency, the pattern of carbon nano-particle, production is individually present in these synthetic methods
Amount and quality are difficult to reach accurate 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 in order to overcome the shortcomings of that above-mentioned there is provided a kind of preparation side of the carbon nano-particle of visible ray supporting Pt
Method, more economic, the convenient and environmental protection when preparing the carbon nano-particle of supporting Pt.
Technical scheme is as follows：
A kind of preparation method of the carbon nano-particle of visible ray supporting Pt, comprises the following steps：
(1) graphite is taken to be put into equipped with H3PW12O40Three-necked flask in, put up reflux, and 3h is stirred at room temperature, so
Flow back 10h under 140 DEG C of fluidized states afterwards；
(2) three-necked flask is cooled to normal temperature, by phegma import 500 type bag filters in, then by the bag filter go from
Permeated in sub- water；
(3) after permeating, the solution in bag filter is adjusted into pH value to 5.5；
(4) above-mentioned solution loading centrifuge tube is centrifuged；
(5) after the completion of centrifuging, supernatant liquor 5ml is taken, 50ml is diluted to deionized water；
(6) step (5) is diluted to obtained solution and imported in Photoreactor and is irradiated；
(7) configuration 0.5ml 0.1M H2PtCl6·6H2O solution, divides 10 times and is added in above-mentioned reactor, adjust at any time
PH value keeps 5.0-6.0；
(8) reaction obtains suspension after terminating, and suspension is dried, and obtains the carbon nanometer of the i.e. supporting Pt of solid particle
Grain.
Wherein, the H that 5M, 150ml are housed in 1g graphite, three-necked flask has been taken in step (1)3PW12O40。
Time of penetration in step (2) is 2 days, and need to change water once per half a day.
In step (3) pH is adjusted using 0.25M NaOH.
With 1500r/min centrifugation 1h in step (4).
Light source in step (6) is high-performance daylight xenon light source, and irradiation time is 360 minutes.
By H in step (7)2PtCl6·6H2The time interval that O solution is added in reactor is 36min.
Drying temperature in step (8) is 40 DEG C, and drying time is 5h.
The beneficial effects of the invention are as follows：
The present invention, which has, continuously to be produced, the advantages of low in the pollution of the environment, when preparing the carbon nano-particle of supporting Pt 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 of supporting Pt；
Fig. 2 is the carbon nano-particle particle diameter test chart of supporting Pt；
Fig. 3 is the SEM figures of raw graphite；
Fig. 4 is the carbon nano-particle TEM figures of supporting Pt；
Fig. 5 is the carbon nano-particle XRD of supporting Pt.
Embodiment
Any feature disclosed in this specification, unless specifically stated otherwise, can be equivalent by other or with similar purpose
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 preparation method of the carbon nano-particle of visible ray supporting Pt, preparation method is as follows：1g graphite is taken, dress is put into
There are 5M, 150ml H3PW12O40Three-necked flask in, put up reflux.3h is stirred at room temperature, then in 140 DEG C of fluidized states
Under, flow back 10h.Treat that three-necked flask is cooled to normal temperature, phegma is imported in 500 type bag filters, the bag filter is in deionized water
Middle infiltration 2 days, during which changes water once per half a day.After infiltration, the solution in bag filter is arrived with 0.25M NaOH regulations pH value
5.5.Above-mentioned solution is loaded into centrifuge tube, 1500r/min is centrifuged 1 hour.After the completion of centrifugation, supernatant liquor 5ml is taken, deionization is used
Water is diluted to 50ml.Above-mentioned solution is imported in homemade Photoreactor, light source is high-performance daylight xenon light source, irradiation 360
Minute.0.5ml 0.1M H are prepared simultaneously2PtCl6·6H2O solution, solution 0.05ml was added every 36 minutes to above-mentioned reaction
In device, 10 solution are added altogether, and pH value is adjusted at any time and keeps 5.0-6.0.Reaction obtains suspension after terminating, and suspension is existed
The carbon nano-particle that the solid particle obtained after 5h, drying is supporting Pt is dried at 40 DEG C.
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, with addition H2PtCl6·6H2The increase of O amounts loads the increase of number of times, on carbon nano-particle
Pt also in increase, curve is more and more steeper, illustrate that Pt has been loaded on carbon nano-particle, but must be every time micro load,
Can the upper Pt of load.In figure, nethermost black bold curve is the carbon nano-particle curve before supporting Pt, it was found from the curve, is
Carbon particle curve.
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 supporting Pt is about 1.2nm, it can thus be concluded that, it is successfully prepared supporting Pt
Carbon nano-particle.
The S4800 type scanning electron microscope sems produced to raw graphite sample by HIT are analyzed (see figure
3) the JEM-1400 type transmission electron microscopes TEM that, solid particle samples obtained above are produced by HIT
Analyzed (see Fig. 4).
As shown in figure 3, lamella aggregation shape is presented in graphite.From shown in Fig. 4, Pt has been loaded on carbon particles, and particle diameter is in 1-
It is consistent with Fig. 2 result between 1.5nm.Compared with Fig. 3, it is known that the lamellar structure of graphite has been destroyed, nanoscale
Carbon particle prepared.
The D8 model X-ray diffractions (X-ray that solid particle samples obtained above are produced by German Brooker company
Diffraction, XRD) analyzed (see Fig. 5).Each parameter is as follows during analysis, CuK α radiation, tube voltage：40kV, tube current：
250mA, 2 θ scanning ranges：10~90 °, sweep speed：4 °/min, scan mode is continuous scanning, temperature：Room temperature (23 DEG C),
Relative humidity：30~40%.
As shown in figure 5, thick black curve is the indicatrix of nano-sized carbon, at 2theta=40, there is a wide sharp peak, be
Pt characteristic peak, illustrates that Pt is successfully loaded on carbon nano-particle.Other small sharp peaks are the impurity remained in sample
Peak.
The invention is not limited in foregoing embodiment.The present invention, which is expanded to, any in this manual to be 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 visible ray supporting Pt, it is characterised in that comprise the following steps：
(1) graphite is taken to be put into equipped with H3PW12O40Three-necked flask in, put up reflux, and 3h is stirred at room temperature, then
Flow back 10h under 140 DEG C of fluidized states；
(2) three-necked flask is cooled to normal temperature, phegma is imported in 500 type bag filters, then by the bag filter in deionized water
Middle infiltration；
(3) after permeating, the solution in bag filter is adjusted into pH value to 5.5；
(4) above-mentioned solution loading centrifuge tube is centrifuged；
(5) after the completion of centrifuging, supernatant liquor 5ml is taken, 50ml is diluted to deionized water；
(6) step (5) is diluted to obtained solution and imported in Photoreactor and is irradiated；
(7) 0.5ml, 0.1M H are prepared2PtCl6·6H2O solution, divides 10 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 is supporting Pt.
2. the preparation method of the carbon nano-particle of supporting Pt according to claim 1, it is characterised in that step takes in (1)
5M, 150ml H are housed in 1g graphite, three-necked flask3PW12O40。
3. the preparation method of the carbon nano-particle of supporting Pt according to claim 1, it is characterised in that in step (2)
Time of penetration is 2 days.
4. the preparation method of the carbon nano-particle of supporting Pt according to claim 1, it is characterised in that step makes in (3)
PH is adjusted with 0.25M NaOH.
5. the preparation method of the carbon nano-particle of supporting Pt according to claim 1, it is characterised in that in step (4) with
1500r/min centrifugation 1h.
6. the preparation method of the carbon nano-particle of supporting Pt according to claim 1, it is characterised in that in step (6)
Light source is high-performance daylight xenon light source, and irradiation time is 360 minutes.
7. the preparation method of the carbon nano-particle of supporting Pt according to claim 1, it is characterised in that will in step (7)
H2PtCl6·6H2The time interval that O solution is added in reactor is 36min.
8. the preparation method of the carbon nano-particle of supporting Pt according to claim 1, it is characterised in that in step (8)
Drying temperature is 40 DEG C, and drying time is 5h.
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