CN107138154A - A kind of Pt@C nano balls - Google Patents
A kind of Pt@C nano balls Download PDFInfo
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- CN107138154A CN107138154A CN201710318738.6A CN201710318738A CN107138154A CN 107138154 A CN107138154 A CN 107138154A CN 201710318738 A CN201710318738 A CN 201710318738A CN 107138154 A CN107138154 A CN 107138154A
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- nano
- balls
- carbon
- platinum
- nano balls
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/42—Platinum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
Abstract
The invention discloses a kind of Pt@C nano balls and preparation method thereof, belong to catalysis technical field.The Pt C nanos ball is using unformed carbon ball as carrier, using glucose, and acetylacetone,2,4-pentanedione platinum is mixed evenly, and the carbon bag platinum core shell structure of cluster-shaped multinuclear is made through one step hydro thermal method in-situ reducing；Advantage of this invention is that the presence of shell carbon-coating forms effective protection to noble metal nano catalyst, it is to avoid the aggregation and oxidation of nanocatalyst.Catalyst preparation process is simple, and activity is high, and stability is good, can be widely applied to p-nitrophenol catalytic hydrogenation and prepares para-aminophenol.
Description
Technical field
The invention belongs to catalysis technical field, more particularly to a kind of Pt@C nano balls.
Background technology
Precious metal material has excellent catalytic performance in itself, and the noble metal granule of nano-scale lacks original due to surface
Son can produce more unsaturated bond, be easier to be combined to balance its surface energy, therefore noble metal nano particles with other atoms
Show higher chemism.Meanwhile, noble metal nano particles are compared with block noble metal, with bigger specific surface area,
That is the ratio of its surface atom exposure is bigger, and exposed avtive spot is more, it is easier to haptoreaction thing, in catalytic reaction application
In, preferably chemical bond rupture or reconstruct can be carried out by catalytic reaction substrate, so as to possess more preferable catalytic activity and Geng Gao
Selectivity.Therefore, have to the research in terms of the development and application of noble metal nanometer material class catalyst highly important
Meaning.
At present, researcher is directed to Pt class catalyst of the exploitation with high catalytic activity and high usage always.With
The size for nano platinum particle reduces, the increase of its specific surface area, and the increase of surface atom number can greatly improve its catalytic performance.But
It is that the nano platinum particle of small size is faced with the problem of can not being stabilized, i.e. high-ratio surface and nano platinum particle can be caused to hold very much
Easily reunite, be easily oxidized.Therefore, the platinum nano catalyst for preparing stable small size is one has the work of challenge very much.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of Pt@C nano balls, this method is simple to operate,
Repeatability is higher.
The purpose of the present invention is achieved through the following technical solutions：A kind of Pt@C nano balls, the Pt@C nano balls
External diameter be 80-120nm, including thickness be 30nm carbon shell, Pt nanoparticle particle diameter about 2-5nm, in cluster-shaped nucleation.Pt@C
The preparation method of nanosphere, this method comprises the following steps：
(1) 1g glucose is dissolved in 20ml deionized waters, adds the acetylacetone,2,4-pentanedione that 0.006g mass fractions are 97%
Powder, moves on to solution in hydrothermal reaction kettle after dispersed with stirring is uniform, hydro-thermal reaction 4h in 180 DEG C；
(2) product centrifuged, washed successively using deionized water and absolute ethyl alcohol, obtaining Pt@C nanos after vacuum drying
Ball.
The beneficial effects of the invention are as follows：The presence of shell carbon-coating is formed with to noble metal nano catalyst in Pt C nano balls
Effect protection, it is to avoid the aggregation and oxidation of nanocatalyst, improves the activity and stability of catalyst.This method operation letter
Single, technological parameter is controllable, and repeatability is very high.And the Pt@C nanos balls prepared are prepared to amino in p-nitrophenol catalytic hydrogenation
Had a wide range of applications in terms of phenol.
Brief description of the drawings
A is the SEM pictures of Pt@C nano balls in Fig. 1, and B, C, D are the TEM pictures of Pt@C nano ball different multiples；
Fig. 2 is the EDS pictures of Pt@C nano balls；
Fig. 3 is the XRD piece of Pt@C nano balls；
Fig. 4 is the scanning electron microscope (SEM) photograph of Pt@C nano ball shell structure forming processes；
Fig. 5 is catalytic effect figure of the Pt@C nanos balls as catalyst.
Embodiment
With reference to specific embodiment, the present invention is furture elucidated.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member makes various changes or modifications to the present invention, and these equivalent form of values equally fall within the model that the application appended claims are limited
Enclose.
Embodiment 1
It is as follows that the present embodiment prepares Pt@C nano ball steps using hydro-thermal method：
1g glucose is dissolved in 20ml deionized waters, the acetylacetone,2,4-pentanedione powder that 0.006g mass fractions are 97% is added
End, moves on to solution in hydrothermal reaction kettle after dispersed with stirring is uniform, hydro-thermal reaction 4h in 180 DEG C；Product is centrifuged, used successively
Pt@C nano balls, such as Figure 1A (scanning electron microscope (SEM) photograph) and Figure 1B, C, D are obtained after deionized water and absolute ethyl alcohol washing, vacuum drying
Shown in (transmission electron microscope picture).
It can be seen that the spherical looks of Pt@C nanos made from hydro-thermal method are uniform from Figure 1A, good dispersion, particle diameter is about 100nm
Left and right.Because platinum Atom of Elements is bigger than the atomic number of carbon and causes two kinds of element contrasts different, thus scanning
It is substantially brighter compared with carbon-coating that electron microscope can see platinum core.The nucleocapsid knot of Pt@C nano balls can be more intuitively observed in Figure 1B
Structure, the nano-cluster that the Pt nano-particles that kernel is 2-5nm are agglomerated into is can see with reference to Fig. 1 C high power transmission electron microscope picture
Structure, diameter is about 50nm or so, and shell is the thick carbon-coatings of about 25nm.It can be seen that obvious brilliant from the D of figure one HRTEM figures
Glazing bar line, and spacing of lattice is 0.23nm, (111) crystal face of correspondence platinum demonstrates nano-cluster composition for platinum element.
Fig. 2 is the EDS spectrograms of Pt@C nano balls, it can be seen that contain Cu element systems in Pt, C element, spectrogram in the structure
Brought into during sample.39 °, 46 °, 68 ° of positions as shown in figure 3, there are three stronger characteristic peaks, matching in the XRD of Pt@C nano balls
Pt standard card (JCPDS card No.04-0802), correspond to respectively face-centred cubic structure platinum (111), (200) and
(220) three diffraction crystal faces.Illustrate that there is the platinum simple substance of cube face-centred cubic structure in prepared Pt C nano balls, this and figure
EDS characterization results in 2 match.
Embodiment 2
The present embodiment studies the forming process of Pt@C nano balls.
It is water insoluble under acetylacetone,2,4-pentanedione platinum normal temperature, therefore can not be carried out under the reaction normal temperature, and HTHP in a kettle.
In the environment of, the platinum ion after dissolving can be reduced to form Pt nanoparticle and further reunite by glucose, as shown in Figure 4 A.With
Proceeding for reaction, glucose can be carbonized, form porous carbon layer and be coated on around platinum nanoclusters, and with reaction
Time continues to increase, and carbon-coating progressive additive ultimately forms the Pt@C nano balls of core shell structure, as shown in Fig. 4 B, C.
Embodiment 3
The Pt@C nanos ball that the present embodiment prepares embodiment 1 is used for the catalytic hydrogenation of nitrophenol, is specially：
Step：Configure 1mol/L NaBH4(reducing agent, reduce p-nitrophenol) solution 2ml, 5.0 × 10-4Mol/L's
P-nitrophenol (4-NP) solution 100ml, takes 4-NP solution and 1ml NaBH4 that 50ml is prepared to be added in 100ml beakers,
After ultrasound is uniform, first takes a sample to carry out UV absorption test, make object of reference.Then 3mg Ag-Pt@C nano balls, ultrasound are added
It is well mixed to carry out UV absorption test.UV absorption test is carried out after 2min samples 2ml, every sub-sampling.
As shown in figure 5, in no addition Pt@C nano catalyst, there is a strong absworption peak in 400nm or so, it is right
Answer the Absorption Characteristics peak of p-nitrophenol.Add after Pt@C nano catalyst, a new peak, correspondence occur in 300nm or so
The characteristic absorption peak of 4- nitroanilines.Increase over time, the characteristic peak of p-nitrophenol is more and more weaker, 4- nitroanilines
Characteristic peak is more and more stronger, and until reaction is carried out after 14min, curve is basicly stable, illustrates that 4-NP is reduced by thorough catalysis.The reality
Pt@C nanos balls that example discloses are applied for degraded organic contamination, have prominent application prospect in terms of processing industrial wastewater.
Claims (1)
1. a kind of Pt@C nano balls, it is characterised in that external diameter is 80-120nm, including the carbon shell that thickness is 30nm, platinum nanometer
Grain particle diameter about 2-5nm, cluster nucleation；Characterized in that, this method is：
(1) 1g glucose is dissolved in 20ml deionized waters, adds 0.006g acetylacetone,2,4-pentanedione powder, will after dispersed with stirring is uniform
Solution is moved on in hydrothermal reaction kettle, hydro-thermal reaction 4h in 180 DEG C；
(2) product centrifuged, washed successively using deionized water and absolute ethyl alcohol, obtaining Pt@C nano balls after vacuum drying.
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| CN201710318738.6A CN107138154A (en) | 2017-05-08 | 2017-05-08 | A kind of Pt@C nano balls |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108970608A (en) * | 2018-07-18 | 2018-12-11 | 南京大学 | Loaded noble metal catalyst with clad structure and preparation method thereof and the application in Cu (II) liquid phase catalytic reduction |
| CN108993485A (en) * | 2018-06-30 | 2018-12-14 | 浙江工业大学 | The preparation method and application of a kind of mesoporous carbon microspherical catalyst of original position carried metal |
| CN109482176A (en) * | 2018-11-02 | 2019-03-19 | 中国科学院重庆绿色智能技术研究院 | Catalyst and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104801724A (en) * | 2015-04-03 | 2015-07-29 | 浙江理工大学 | Ag/C (Silver/Carbon) hollow nano-sphere and preparation method thereof |
-
2017
- 2017-05-08 CN CN201710318738.6A patent/CN107138154A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104801724A (en) * | 2015-04-03 | 2015-07-29 | 浙江理工大学 | Ag/C (Silver/Carbon) hollow nano-sphere and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| BAOZHEN LI ET AL.: ""Preparation of Multiple-Pt-nanoclustes-C-shell Nanostructures and Their Catalytic Properties"", 《2016 INTERNATIONAL CONFERENCE ON MATERIAL SICNECE AND CIVIL ENGINEERING》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108993485A (en) * | 2018-06-30 | 2018-12-14 | 浙江工业大学 | The preparation method and application of a kind of mesoporous carbon microspherical catalyst of original position carried metal |
| CN108993485B (en) * | 2018-06-30 | 2021-07-27 | 浙江工业大学 | Preparation method and application of in-situ supported metal mesoporous carbon microsphere catalyst |
| CN108970608A (en) * | 2018-07-18 | 2018-12-11 | 南京大学 | Loaded noble metal catalyst with clad structure and preparation method thereof and the application in Cu (II) liquid phase catalytic reduction |
| CN109482176A (en) * | 2018-11-02 | 2019-03-19 | 中国科学院重庆绿色智能技术研究院 | Catalyst and preparation method thereof |
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Application publication date: 20170908 |