CN111569871B - Preparation method of flower-shaped structure platinum nano material - Google Patents
Preparation method of flower-shaped structure platinum nano material Download PDFInfo
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- CN111569871B CN111569871B CN202010462114.3A CN202010462114A CN111569871B CN 111569871 B CN111569871 B CN 111569871B CN 202010462114 A CN202010462114 A CN 202010462114A CN 111569871 B CN111569871 B CN 111569871B
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 80
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 38
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 36
- 150000003839 salts Chemical class 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 229910013553 LiNO Inorganic materials 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 150000002894 organic compounds Chemical class 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000002844 melting Methods 0.000 claims abstract description 4
- 230000008018 melting Effects 0.000 claims abstract description 4
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 3
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 4
- -1 polytetrafluoroethylene Polymers 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims 1
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 15
- 239000003054 catalyst Substances 0.000 abstract description 9
- 239000003960 organic solvent Substances 0.000 abstract description 6
- 239000003223 protective agent Substances 0.000 abstract description 6
- 230000003197 catalytic effect Effects 0.000 abstract description 5
- 238000006555 catalytic reaction Methods 0.000 abstract description 4
- 239000003795 chemical substances by application Substances 0.000 abstract description 4
- 239000004094 surface-active agent Substances 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 description 5
- 239000002608 ionic liquid Substances 0.000 description 5
- 239000002057 nanoflower Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229910021098 KOH—NaOH Inorganic materials 0.000 description 3
- 239000000446 fuel Substances 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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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
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/58—Platinum group metals with alkali- or alkaline earth metals
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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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/88—Processes of manufacture
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
- H01M4/90—Selection of catalytic material
- H01M4/92—Metals of platinum group
- H01M4/921—Alloys or mixtures with metallic elements
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/50—Fuel cells
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Abstract
The invention belongs to the technical field of preparation of platinum nano materials, and aims to solve the problem that the preparation of the platinum nano materials uses an organic solvent and an organic protective agent, which causes serious harm to the environment and human health; high price and non-cyclability, is not beneficial to the problems of large-scale production, commercial application and the like, provides a preparation method of a flower-shaped platinum nano material, and uses KNO 3 ‑LiNO 3 And (2) taking the mixed salt bath as a heating source, uniformly mixing KOH and NaOH, completely melting at 180 ℃, adding an organic compound of platinum while stirring, heating to 200 or 230 ℃, reacting for 3 hours, naturally cooling, adding distilled water to dissolve solid salt, repeatedly performing centrifugal separation, washing with distilled water, and drying to obtain the flower-shaped platinum nano material. The preparation process does not use any organic surfactant and structure directing agent, the product surface is very clean, the product is directly used in electrochemical catalysis, has very high ORR and methanol electrochemical catalytic activity, and has very great application prospect in the fields of catalyst preparation and application.
Description
Technical Field
The invention belongs to the technical field of preparation of platinum nano materials, and particularly relates to a preparation method of a flower-shaped platinum nano material.
Background
The noble metal platinum nano material has excellent electro-catalytic performance and is widely used as a catalyst for anode oxidation and cathode oxygen reduction reactions of fuel cells. The performance of the catalyst is closely related to the structure, composition, morphology, surface atomic distribution, size and the like of the catalyst, and the prepared platinum and platinum-based alloy with proper size, specific morphology and excellent catalytic performance can greatly reduce the cost of the fuel cell and promote the popularization and application of the fuel cell.
At present, the preparation of platinum nano-materials is mostly carried out in a water phase or an oil phase, and a surfactant or a structure directing agent is added to prevent the aggregation of nano-particles and guide the growth of nano-crystals. However, the use of organic solvents and organic protective agents has many problems, and most of the organic solvents with high toxicity and volatility can cause serious harm to the environment and human health; organic protective agent molecules adsorbed on the surfaces of catalyst particles are not easy to remove, and impurities can cause adverse effects on the surface activity of the catalyst; in addition, the high price and non-recyclability of the organic solvent and the organic protective agent are not favorable for the scale production and the commercial application of the catalyst. Therefore, the development of a simple, convenient and environment-friendly preparation method which does not use volatile and toxic organic solvents and organic protective agents which are difficult to clean has great significance.
Disclosure of Invention
Aiming at the problems, the invention provides a preparation method of a flower-shaped platinum nano material, which is used for preparing the flower-shaped platinum nano material in KOH-NaOH molten salt inorganic ionic liquid. In the preparation process, no organic solvent or organic protective agent is used, so that the environment is not polluted, and the prepared nanoparticles have clean surfaces and high catalytic activity. Meanwhile, the inorganic ionic liquid can be recycled and reused for many times, and the method is a widely-used green method for preparing the nano material.
In order to achieve the purpose, the invention is realized by the following technical scheme: a preparation method of a flower-shaped structure platinum nano material comprises the following steps: mixing KOH and NaOH, and KNO 3 -LiNO 3 And (2) taking the mixed salt bath as a heating source, completely melting the NaOH-KOH mixed salt at 180 ℃, adding an organic compound of platinum at 180 ℃ under the stirring state, heating to 200 ℃ or 230 ℃, reacting for 3 hours, stopping the reaction, naturally cooling, adding distilled water to dissolve solid salt, repeatedly centrifuging, separating, washing with distilled water, and drying to obtain the flower-shaped structure platinum nano material.
The weight ratio of the KOH to the NaOH is as follows: n is KOH :n NaOH = 0.485; grinding KOH and NaOH, mixing uniformly, adding the mixture into a polytetrafluoroethylene inner lining, completely melting NaOH-KOH mixed salt at 180 ℃, and then controlling the stirring speed to be 800-1000 r/min.
The organic compound of platinum is tetraammine oxalate complex of platinum, i.e.Pt(NH 3 ) 2 C 2 O 4 The amount added was 0.05 mM. The centrifuged upper layer liquid can be recovered and can be reused after recrystallization.
The method is very simple and convenient, and no organic surfactant or structure directing agent is used in the preparation process, so that the method is completely green and environment-friendly. In the experiment, KOH-NaOH molten salt inorganic ionic liquid is used as a reaction solvent, and the KOH-NaOH molten salt inorganic ionic liquid is correspondingly matched according to the lowest eutectic point (mass ratio n) KOH :n NaOH = 0.485), the mixed inorganic systems melt into liquid at the eutectic point of 170 ℃, the strong alkalinity of the mixed inorganic systems promotes the thermal decomposition of the noble metal organic precursors at a lower temperature, and the ionic characteristics of the inorganic ionic liquid enable the generated nano particles to stably exist without agglomeration. The preparation process does not use any organic surfactant and structure-directing agent, so the product surface is very clean, the product is directly used in electrochemical catalysis without any pretreatment before use, and the methanol electrochemical catalysis has very high methanol electrochemical catalysis activity and has very wide application prospect in the fields of catalyst preparation and application.
Drawings
FIG. 1 is a scanning and transmission electron microscope image and XRD spectrum of a platinum nanoflower-like structure prepared at 200 ℃ in example 1; in the figure: a and b are scanning electron micrographs under 1 mu m and 200nm respectively; c, d and e are transmission electron microscope images at 50nm, 10nm and 2nm respectively; f is an XRD spectrogram;
FIG. 2 is a scanned image of platinum nanoflower-like structures prepared at 230 ℃ in example 2.
Detailed Description
Example 1: grinding 4.12g KOH and 5.44 g NaOH, mixing, adding into polytetrafluoroethylene inner lining, and using KNO 3 -LiNO 3 The mixed salt bath is used as a heating source to completely melt the NaOH-KOH mixed salt at 180 ℃, the stirring speed is kept to be 1000-8000 rpm, 17.6 mg of tetraammineplatinum oxalate is added at 180 ℃, the temperature is raised to 200 ℃, the reaction is continued for 3 hours, the reaction is stopped, distilled water is added after the reaction is cooled to dissolve solid salt, and the platinum nano flower-shaped structure is obtained through centrifugal separation, multiple times of cleaning and drying.
As shown in FIG. 1, the scanning photograph of a shows that the product is composed of nanometer flower-like structures with uniform size, and the further enlarged scanning photograph shows that the nanometer flower size is about 400-500 nm (b). c-e is a transmission photo of the platinum nanoflower, the platinum nanoflower is seen to be composed of a central stamen and dendritic petals scattered towards the periphery from the c picture, and an enlarged transmission photo (d picture) shows that the petals of the platinum nanoflower are composed of a plurality of small nanosheets growing together along the long-branch direction. As can be seen from the high-resolution transmission photograph (e picture) of the lattice phase, the interplanar spacing between adjacent lattice lines is 0.223 nm, which corresponds to the platinum (111) crystal face of the face-centered cubic structure, and the lattice orientations are highly consistent in the same nanosheet. The diffraction peaks in the XRD diffraction pattern of the platinum nanoflower in the f picture respectively correspond to the standard diffraction peaks of the (111), (200), (220), (311) and (222) crystal faces of the platinum with the face-centered cubic structure, and no other impurity diffraction peaks exist, so that the prepared platinum nanoflower is pure platinum with the face-centered cubic structure.
The product was used as an anode catalyst for catalytic oxidation of methanol, and CV test was carried out in perchloric acid solution (0.1M) by the three-electrode method, and the active surface area thereof was 3.64M 2 G, area activity 1.23 mA/cm 2 @0.9V, 1.08 mA/cm higher than commercial platinum black 2 @0.9V, indicating that the product has high electrochemical catalytic activity for methanol oxidation.
Example 2: grinding 4.12g KOH and 5.44 g NaOH, mixing, adding into polytetrafluoroethylene inner lining, and using KNO 3 -LiNO 3 The mixed salt bath is used as a heating source to completely melt the NaOH-KOH mixed salt at 180 ℃, the stirring speed is kept to be 1000-8000 rpm, 17.6 mg of tetraammineplatinum oxalate is added at 180 ℃, the temperature is raised to 230 ℃, the reaction is continued for 3 hours, the reaction is stopped, distilled water is added after the reaction is cooled to dissolve solid salt, and the product is obtained by centrifugal separation, multiple times of cleaning and drying.
As shown in fig. 2, it can be seen that the product is a sunflower-like flower-like platinum nanostructure, the size of which is around 2-3.5 μm.
Claims (2)
1. Preparation method of flower-shaped structure platinum nano materialThe method is characterized in that: the method comprises the following steps: mixing KOH and NaOH, and KNO 3 -LiNO 3 The mixed salt bath is a heating source, naOH-KOH mixed salt is completely melted at 180 ℃, an organic compound of platinum is added at 180 ℃ under the stirring state, the temperature is raised to 200 ℃ or 230 ℃, the reaction is carried out for 3 hours, after the reaction is stopped, the natural cooling is carried out, distilled water is added to dissolve solid salt, and the centrifugal separation, the cleaning with the distilled water and the drying are carried out repeatedly to obtain the flower-shaped structure platinum nano material;
the mass ratio of KOH and NaOH is as follows: n is a radical of an alkyl radical KOH :n NaOH = 0.485; grinding KOH and NaOH, mixing uniformly, adding the mixture into a polytetrafluoroethylene inner lining, completely melting NaOH-KOH mixed salt at 180 ℃, and then controlling the stirring speed to be 800-1000 r/min.
2. The method for preparing the platinum nanomaterial with the flower-like structure according to claim 1, wherein the method comprises the following steps: the organic compound of platinum is tetraammine oxalate complex of platinum, i.e. Pt (NH) 3 ) 2 C 2 O 4 The amount added was 0.05 mM.
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| CN101406832A (en) * | 2008-11-24 | 2009-04-15 | 中国科学院长春应用化学研究所 | Method for preparing monodisperse flower-shaped gold/platinum hybrid nano particles having different particle diameters |
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| CN101519191B (en) * | 2009-03-31 | 2010-12-08 | 中国科学院新疆理化技术研究所 | Method for preparing oxide nano-materials by melted hydrated salt |
| CN101791702B (en) * | 2010-03-04 | 2011-07-27 | 西安交通大学 | Method for preparing nano sheets of platinum |
| CN102172539B (en) * | 2011-03-17 | 2012-10-24 | 南京师范大学 | Method for preparing platinum nano cluster catalyst through thermal decomposition of complex |
| CN106540713A (en) * | 2016-11-03 | 2017-03-29 | 北京工业大学 | A kind of original position prepares the molte-salt synthesis of iron sesquioxide loading platinum nanocatalyst |
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| CN101406832A (en) * | 2008-11-24 | 2009-04-15 | 中国科学院长春应用化学研究所 | Method for preparing monodisperse flower-shaped gold/platinum hybrid nano particles having different particle diameters |
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