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A method for the preparation of novel non-noble metal electrocatalysts by co-assembly of double porphyrins

A non-precious metal and electrocatalyst technology, which is applied in the field of bis-porphyrin co-assembly to prepare a new type of non-precious metal electrocatalyst, which can solve the problems of large sheet structure size and unfriendly environment, and achieve the effects of diverse performance, environmental friendliness and novel structure

Active Publication Date: 2018-11-09
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In 2010, Professor Shelnutt and other researchers studied and prepared nanostructures with four-leaf clover morphology (J.Am.Chem.Soc.2010,132,8194–8201). In the process of synthesizing anion zinc porphyrin, the methanol and chloroform solution, the reaction solvent is not friendly to the environment
In 2012, this group of researchers further used the negative ion zinc porphyrin and positive ion tin porphyrin to prepare a micro-nano scale sheet structure (Nanoscale, 2012, 4, 1695–1700). The sheet structure obtained in this report The size is large, and the scope of application has certain limitations

Method used

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  • A method for the preparation of novel non-noble metal electrocatalysts by co-assembly of double porphyrins
  • A method for the preparation of novel non-noble metal electrocatalysts by co-assembly of double porphyrins
  • A method for the preparation of novel non-noble metal electrocatalysts by co-assembly of double porphyrins

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: the preparation of nano flower

[0038] At 25°C, mix 10 mL of 5 mM solution of MESO-tetrakis(4-sulfonate)porphyrin iron with 10 mL of 5 mM solution of MESO-tetrakis(4-methyl-4-pyridyl)porphyrin iron, and stir After 20min, let it stand for 2 days, suction filter and dry, the obtained product was heat-treated under argon at 775°C, and then heated with 0.5M H at 80°C 2 SO 4 The solution was washed for 30 min, then washed with water until neutral, and dried to obtain a non-precious metal electrocatalyst.

[0039] As shown in Figure 1 (a), (b), a kind of MESO-tetra(4-sulfonic acid group) porphyrin iron and MESO-tetrakis (4-methyl-4-pyridyl) porphyrin iron used in Example 1 the structural formula.

[0040] Such as figure 2 , the TEM transmission electron microscope shows a nanoflower structure, and the average size distribution of the outer diameter of the nanoflower is 300-400nm.

[0041] Such as image 3 , Comparison of the oxygen reduction activity of t...

Embodiment 2

[0045] Embodiment 2: Reaction temperature is different: the preparation of nano flower

[0046] At 0°C, mix 10 mL of 5 mM solution of MESO-tetrakis(4-sulfonate)porphyrin iron with 10 mL of 5 mM solution of MESO-tetrakis(4-methyl-4-pyridyl)porphyrin iron, and stir After 20min, let it stand for 2 days, suction filter and dry, the obtained product was heat-treated under argon at 775°C, and then heated with 0.5M H at 80°C 2 SO 4 The solution was washed for 30 min, then washed with water until neutral, and dried to obtain a non-precious metal electrocatalyst.

[0047] Such as Figure 7 , the TEM transmission electron microscope shows a nanoflower structure, and the average size distribution of the outer diameter of the nanoflower is 300-400nm.

[0048] Such as Figure 8 , the oxygen reduction activity comparison chart of non-noble metal electrocatalyst prepared in embodiment 2 and commercial Pt / C in 0.1M KOH solution. The as-prepared non-noble metal electrocatalyst exhibited a...

Embodiment 3

[0052] Embodiment 3: add surfactant: the preparation of nano half bowl

[0053] At 25°C, mix 10 mL of 5mM MESO-tetrakis(4-methyl-4-pyridyl)porphyrin iron solution with 10 mL of 5mM MESO-tetrakis(4-sulfonate) mixed with 2mM 5mL sodium dodecyl sulfate solution Acid-based) porphyrin iron solution and mix, after stirring for 20min, let it stand for 2 days, suction filter and dry, the product obtained was heat-treated at 775°C under argon, and then heated with 0.5MH at 80°C 2 SO 4 The solution was washed for 30 min, then washed with water until neutral, and dried to obtain a non-precious metal electrocatalyst.

[0054] Such as Figure 12 , a TEM transmission electron microscope shows a nanoflower structure, and the average size distribution of the outer diameter of the nanometer half-bowl structure is 300-400nm.

[0055] Such as Figure 13 , Comparison of the oxygen reduction activity of the non-noble metal electrocatalyst prepared in Example 3 and commercial Pt / C in 0.1M KOH s...

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Abstract

The invention belongs to the field of preparation of a nanometer material and provides a method for assembling and preparing a novel non-precious metal electrocatalyst through bisporphyrin. The method is used for controllably preparing the feature of the non-precious metal electrocatalyst and further adjusting and changing the electrochemical activity and stability thereof. The method comprises the following steps: directly mixing a porphyrin solution dissolving positive ions and a porphyrin solution dissolving negative ions at equal concentration and equal volume, or firstly mixing the porphyrin solution dissolving one electric charge with a surface active agent solution with same electric charge, and then adding the porphyrin solution dissolving opposite charges in same quantity of electric charges; acquiring a material with a certain feature; roasting at high temperature; after pickling, basically maintaining the feature of the material. The synthetic method provided by the invention has the advantages of universality, simpleness, high speed, capability of effectively regulating the feature of the non-precious metal electrocatalyst and further adjusting and changing the electrochemical activity and stability of the non-precious metal electrocatalyst, and application to the fuel cells.

Description

technical field [0001] The invention belongs to the field of preparation of nanometer materials, and relates to a method for co-assembling double porphyrins to prepare a novel non-noble metal electrocatalyst. Background technique [0002] Porphyrins and metalloporphyrin macrocyclic compounds can self-assemble into various ordered nanostructures with various shapes through weak interactions such as hydrogen bonds, van der Waals forces, electrostatic attraction, coordination bonds, or Π-Π stacking interactions. These porphyrin nanostructures have excellent photoelectric properties, and have great application potential in artificially simulated photosynthesis, dye-sensitized solar cells, catalysts, and sensors. However, the structure obtained by the self-assembly between single porphyrin molecules is relatively simple, and the performance shown is often not completely satisfactory. Therefore, people shift the research focus to the co-assembly of multiple porphyrins. The prefer...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B82Y30/00
CPCB01J31/183B01J31/22B82Y30/00
Inventor 宋玉江谢妍
Owner DALIAN UNIV OF TECH