CN101791702A - Method for preparing nano sheets of platinum - Google Patents
Method for preparing nano sheets of platinum Download PDFInfo
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- CN101791702A CN101791702A CN 201010117232 CN201010117232A CN101791702A CN 101791702 A CN101791702 A CN 101791702A CN 201010117232 CN201010117232 CN 201010117232 CN 201010117232 A CN201010117232 A CN 201010117232A CN 101791702 A CN101791702 A CN 101791702A
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Abstract
The invention discloses a method for preparing nano sheets of platinum, which comprises the following steps: adding sodium tripolyphosphate into a mixed melted salt system of sodium hydroxide and potassium hydroxide, adding solid powder of an organic compound of platinum into the mixed melt and violently stirring until the mixed melt is fully reacted; and standing and preserving the heat for some time, after cooling, washing the mixture with water for a plurality of times and performing centrifugal separation on the mixture to obtain a product, namely the nano sheets of platinum. The whole preparation process has convenient operation and simple process and can be applied to the massive preparation of nano sheet structures of noble metal platinum. The melted salt of sodium hydroxide and potassium hydroxide used in the method can be reclaimed, so the method causes no pollution to the environment and has a low cost. The thickness of the obtained nano sheets is 20nm and the size of the obtained nano sheets is between 0.8 and 2.8 mu m and can be adjusted through reaction time and temperature. The nano sheet is of polycrystalline two-dimensional plane structure formed by interconnecting platinum nano particles and has high specific surface and surface selective catalytic activity, so the nano sheets of platinum have vast application prospect.
Description
Technical field
The present invention relates to a kind of preparation method of nano sheets of platinum, particularly a kind ofly interconnect and the preparation method of the polycrystalline two-dimensional plane laminated structure nanometer sheet formed by nano platinum particle.
Background technology
Because the noble metal platinum nanocrystal has high specific area and surface catalysis activity, CO catalytic oxidation, fuel cell reaction, nitration reaction, petroleum cracking etc. there is unusual unique catalytic action, it also can be used as stable electrode material simultaneously, so receive very big concern in the application in fields such as energy catalysis always.
The catalytic property that studies confirm that metal nanocrystal depends on physical quantitys such as its size, shape, composition, structure, can obtain needed performance by regulating above physical quantity usually.At present the research of noble metal platinum nanocrystal mainly is devoted to change its shape, structure and size etc., thereby realize the increase of specific area and surface catalysis activity, the primary study particular crystal plane is to the selection catalytic activity of specific reaction, { the 100} and { 210} crystal face can distinguish selectivity catalysis H nanocrystalline as Pt
2Reaction with CO.
But so far, to not seeing report in the synthetic report of the preparation of the platinum nanocrystal of special shape about the polycrystalline two-dimensional plane laminated structure.Simultaneously at present one all is to adopt to carry out in the organic reaction system of complexity to the preparation of metal nanocrystal, the preparation process complexity, reaction dissolvent can not reclaim repeated use, easily environment is caused very big pollution, be unfavorable for large-scale production, therefore limited its application greatly in fields such as catalysis.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, provide a kind of preparation technology simple, the recyclable repeated use of used flux, pollution-free, with low cost, can realize the method for prepared in batches nano sheets of platinum.The nano sheets of platinum of making by preparation method of the present invention interconnects the polycrystalline two-dimensional plane structure of forming by nano platinum particle, has very big specific surface and surface selection catalytic activity, thereby has great application prospect at catalytic field.
For achieving the above object, the technical solution used in the present invention is: 1) at first, grind to form fine powder after NaOH and potassium hydroxide mixed by 1.06: 1 mass ratio, fine powder heat fused after will grinding then is a liquation, under agitation sodium polyphosphate is joined in the fused solution after dissolving, under 200～230 ℃, leave standstill insulation and got mixed molten liquid in 0.5～1 hour, then the organic compound pressed powder of platinum being joined the mass concentration that makes the organic compound of platinum in the above-mentioned mixed melting liquid is 0.2%, vigorous stirring is until abundant reaction, leave standstill insulation and got mixed liquor in 2～16 hours under 200～230 ℃, wherein the mass ratio of the organic compound of the platinum of Jia Ruing and sodium polyphosphate is 1: 1～3; 2) after reaction finishes mixed liquor is cooled to room temperature and solidifies, water dissolves and centrifugation, and the product that obtains after sediment is repeatedly washed is the nanometer sheet of platinum.
The organic compound of platinum of the present invention is that the acetylacetonate compound of platinum is Pt (acac)
2
Whole process of preparation of the present invention is easy to operate, and technology is simple, can be used for a large amount of preparations of the nano-sheet structure of noble metal platinum.Used fused salt NaOH of this method and the recyclable repeated use of potassium hydroxide, pollution-free, with low cost, the thickness of the nanometer sheet that is obtained is about 20nm, and size is between 0.8 μ m-2.8 μ m, and the size of size can be regulated by reaction time and temperature.This nanometer sheet interconnects the polycrystalline two-dimensional plane structure of forming by nano platinum particle, has very big specific surface and surface selection catalytic activity, thereby has great application prospect at catalytic field.
Description of drawings
Fig. 1 is the nano sheets of platinum scanning electron microscope image of embodiment 1 preparation; Fig. 2 is the nano sheets of platinum images of transmissive electron microscope of embodiment 1 preparation.
The specific embodiment
Below in conjunction with drawings and Examples the present invention is described in further detail.
Embodiment 1: at first, the NaOH that with gross mass is 10g becomes fine powder with the potassium hydroxide mixed grinding, wherein the mass ratio of NaOH and potassium hydroxide is 1.06: 1, fine powder heat fused after will grinding then is a liquation, under agitation sodium polyphosphate is joined in the fused solution after dissolving, leave standstill insulation and got mixed molten liquid in 0.5 hour under 230 ℃, the acetylacetonate compound with platinum is Pt (acac) then
2It is Pt (acac) that pressed powder joins the acetylacetonate compound that makes platinum in the above-mentioned mixed melting liquid
2Mass concentration be 0.2%, vigorous stirring is until abundant reaction, under 200 ℃, leave standstill insulation 5 hours mixed liquor, wherein the mass ratio of the organic compound of the platinum of Jia Ruing and sodium polyphosphate is 1: 3; After reaction finishes mixed liquor is cooled to room temperature and solidifies, water dissolves and centrifugation, and the product that obtains after sediment is repeatedly washed is the nano sheets of platinum of size between 0.8 μ m～1.2 μ m.The nano sheets of platinum diameter of the present invention's preparation is between 0.8 μ m～1.2 μ m as seen from Figure 1, and the nano sheets of platinum of the present invention's preparation is polycrystalline structure as seen from Figure 2.
Embodiment 2: at first, the NaOH that with gross mass is 10g becomes fine powder with the potassium hydroxide mixed grinding, wherein the mass ratio of NaOH and potassium hydroxide is 1.06: 1, fine powder heat fused after will grinding then is a liquation, under agitation sodium polyphosphate is joined in the fused solution after dissolving, leave standstill insulation and got mixed molten liquid in 1 hour under 200 ℃, the acetylacetonate compound with platinum is Pt (acac) then
2It is Pt (acac) that pressed powder joins the acetylacetonate compound that makes platinum in the above-mentioned mixed melting liquid
2Mass concentration be 0.2%, vigorous stirring is until abundant reaction, under 200 ℃, leave standstill insulation 16 hours mixed liquor, wherein the mass ratio of the organic compound of the platinum of Jia Ruing and sodium polyphosphate is 1: 2; After reaction finishes mixed liquor is cooled to room temperature and solidifies, water dissolves and centrifugation, and the product that obtains after sediment is repeatedly washed is the nano sheets of platinum of size between 2.2 μ m～2.8 μ m.
Embodiment 3: at first, the NaOH that with gross mass is 10g becomes fine powder with the potassium hydroxide mixed grinding, wherein the mass ratio of NaOH and potassium hydroxide is 1.06: 1, fine powder heat fused after will grinding then is a liquation, under agitation sodium polyphosphate is joined in the fused solution after dissolving, leave standstill insulation and got mixed molten liquid in 1 hour under 215 ℃, the acetylacetonate compound with platinum is Pt (acac) then
2It is Pt (acac) that pressed powder joins the acetylacetonate compound that makes platinum in the above-mentioned mixed melting liquid
2Mass concentration be 0.2%, vigorous stirring is until abundant reaction, under 230 ℃, leave standstill insulation 2 hours mixed liquor, wherein the mass ratio of the organic compound of the platinum of Jia Ruing and sodium polyphosphate is 1: 1; After reaction finishes mixed liquor is cooled to room temperature and solidifies, water dissolves and centrifugation, and the product that obtains after sediment is repeatedly washed is the nano sheets of platinum of size between 1.2 μ m～1.8 μ m.
Claims (2)
1. the preparation method of a nano sheets of platinum is characterized in that:
1) at first, grind to form fine powder after NaOH and potassium hydroxide mixed by 1.06: 1 mass ratio, fine powder heat fused after will grinding then is a liquation, under agitation sodium polyphosphate is joined in the fused solution after the fusing, under 200～230 ℃, leave standstill insulation and got mixed molten liquid in 0.5～1 hour, then the organic compound pressed powder of platinum being joined the mass concentration that makes the organic compound of platinum in the above-mentioned mixed melting liquid is 0.2%, vigorous stirring is until abundant reaction, leave standstill insulation and got mixed liquor in 2～16 hours under 200～230 ℃, wherein the mass ratio of the organic compound of the platinum of Jia Ruing and sodium polyphosphate is 1: 1～3;
2) after reaction finishes mixed liquor is cooled to room temperature and solidifies, water dissolves and centrifugation, and the product that obtains after sediment is repeatedly washed is the nanometer sheet of platinum.
2. the preparation method of nano sheets of platinum according to claim 1, it is characterized in that: the organic compound of said platinum is that the acetylacetonate compound of platinum is Pt (acac)
2
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| CN2010101172327A CN101791702B (en) | 2010-03-04 | 2010-03-04 | Method for preparing nano sheets of platinum |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211201A (en) * | 2011-05-16 | 2011-10-12 | 西安交通大学 | Method for preparing Pt, Pd and Pt-M (M is Cu, Ag and Pd) alloy nanoparticles |
| CN102728849A (en) * | 2012-05-08 | 2012-10-17 | 清华大学 | Self-supporting noble metal nanosheet with equal thickness of monatomic layer and preparation method of nanosheet |
| CN103466688A (en) * | 2013-09-17 | 2013-12-25 | 中国科学院福建物质结构研究所 | Method for preparing ZnS nanosheet |
| CN111569871A (en) * | 2020-05-27 | 2020-08-25 | 山西大同大学 | Preparation method of flower-shaped structure platinum nano material |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299720A (en) * | 1999-12-13 | 2001-06-20 | 中国科学院化学研究所 | Preparation of nanometer-level platinum metal cluster |
| CN101345111A (en) * | 2008-05-20 | 2009-01-14 | 湖南工业大学 | Novel method of manufacturing Fe3O4/Pt magnetic complex nano particle |
-
2010
- 2010-03-04 CN CN2010101172327A patent/CN101791702B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1299720A (en) * | 1999-12-13 | 2001-06-20 | 中国科学院化学研究所 | Preparation of nanometer-level platinum metal cluster |
| CN101345111A (en) * | 2008-05-20 | 2009-01-14 | 湖南工业大学 | Novel method of manufacturing Fe3O4/Pt magnetic complex nano particle |
Non-Patent Citations (1)
| Title |
|---|
| 《React.Kinet.Catal.Lett.》 20041231 Xiao-Xiang Han et al. HYDROGENATION CATALYSTS BASED ON PLATINUM COMPLEXES WITH POLYMER 41-47 1-2 第81卷, 第1期 2 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102211201A (en) * | 2011-05-16 | 2011-10-12 | 西安交通大学 | Method for preparing Pt, Pd and Pt-M (M is Cu, Ag and Pd) alloy nanoparticles |
| CN102211201B (en) * | 2011-05-16 | 2012-11-28 | 西安交通大学 | Method for preparing Pt, Pd and Pt-M (M is Cu, Ag and Pd) alloy nanoparticles |
| CN102728849A (en) * | 2012-05-08 | 2012-10-17 | 清华大学 | Self-supporting noble metal nanosheet with equal thickness of monatomic layer and preparation method of nanosheet |
| CN102728849B (en) * | 2012-05-08 | 2013-09-18 | 清华大学 | Self-supporting noble metal nanosheet with equal thickness of monatomic layer and preparation method of nanosheet |
| CN103466688A (en) * | 2013-09-17 | 2013-12-25 | 中国科学院福建物质结构研究所 | Method for preparing ZnS nanosheet |
| CN111569871A (en) * | 2020-05-27 | 2020-08-25 | 山西大同大学 | Preparation method of flower-shaped structure platinum nano material |
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| CN101791702B (en) | 2011-07-27 |
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