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N, P double-doped graphitized carbon material based on self-assembled nanometer material of metalloporphyrin and phosphazene, preparation method and application thereof

A technology of metalloporphyrins and nanomaterials, applied in the fields of material chemistry and electrochemistry, to achieve high yield, good conductivity, and regular shape

Active Publication Date: 2019-06-14
HENAN UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, since the research on P doping has just started, the controlled synthesis of N and P double doped carbon materials still needs further research.

Method used

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  • N, P double-doped graphitized carbon material based on self-assembled nanometer material of metalloporphyrin and phosphazene, preparation method and application thereof
  • N, P double-doped graphitized carbon material based on self-assembled nanometer material of metalloporphyrin and phosphazene, preparation method and application thereof
  • N, P double-doped graphitized carbon material based on self-assembled nanometer material of metalloporphyrin and phosphazene, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0050] A preparation method based on porphyrin and phosphazene co-assembly N, P double-doped graphitized carbon material, comprising the following steps:

[0051] (1) Weigh 100 mg (0.15 mmol) of THPP, add 183 mg (0.75 mmol) of cobalt acetate, grind and mix well, place in a 50 mL round bottom flask, add 30 mL of DMF as a solvent, ultrasonicate for 5 min, and put in a magnet React in an oil bath at 45°C for 1 h, pour into deionized water after the reaction, store in the refrigerator at -25°C for 12 h, centrifuge and wash until the supernatant is colorless, freeze at -71°C Dry for 5-10 h for later use to obtain Co-THPP;

[0052] (2) Take 10 mg (0.0135 mmol) of the synthesized Co-THPP and 10 mg (0.0288 mmol) of HCCP, add 30 mL of acetonitrile, and perform ultrasonication at a constant temperature of 20 °C for 20 min in an ultrasonic cleaner;

[0053] (3) Add 1.0 mL TEA to the reaction mixture, continue to sonicate at 20°C for 30 min, centrifuge at 8000 r / min for 10 min, pour off ...

Embodiment 2

[0059] A preparation method based on porphyrin and phosphazene co-assembled N, P double-doped graphitized carbon material, the difference from Example 1 is: take the synthetic tetraphenylhydroxy manganese porphyrin MnTHPP according to Example 1 and HCCP Reaction, tetraphenylhydroxy manganese porphyrin and phosphazene self-assembled nanomaterials are obtained. Then heat treatment according to Example 1 to obtain Mn, N, P double-doped graphitized carbon material.

[0060] SEM images of tetraphenylhydroxymanganese porphyrin and phosphazene self-assembled nanomaterials Figure 4As shown, it can be seen that the material presents a uniform spherical shape with a size of about 246 nm. Obtaining Mn, N, P double-doped graphitized carbon material is carried out oxygen reduction test according to the condition in embodiment 1, and test material has shown better oxygen reduction property, as Figure 13 As shown, the CV (cyclic voltammetry) test results show that in the pass N 2 After...

Embodiment 3

[0062] A kind of preparation method based on porphyrin and phosphazene co-assembly N, P double-doped graphitized carbon material, the difference from Example 1 is: take synthetic tetraphenylnickelyloxyporphyrin NiTHPP according to Example 1 and HCCP Reaction, tetraphenylnickelyl porphyrin and phosphazene self-assembled nanomaterials are obtained. Then heat treatment according to Example 1 to obtain Ni, N, P double-doped graphitized carbon material.

[0063] SEM images of tetraphenylnickelyl porphyrin and phosphazene self-assembled nanomaterials Figure 5 As shown, it can be seen that the material presents a uniform spherical shape with a size of about 80-120 nm. Obtaining Ni, N, P double-doped graphitized carbon material is carried out oxygen reduction test according to the condition in embodiment 1, and test material has shown better oxygen reduction property, as Figure 14 As shown, the CV (cyclic voltammetry) test results show that in the pass N 2 After 20min, Ni, N, P ...

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Abstract

A N, P double-doped graphitize carbon material based on a self-assembled nanometer material of metalloporphyrin and phosphazene, a preparation method and application thereof are disclosed. At first, the self-assembled nano-material of metalloporphyrin and phosphazene are prepared by self-assembling, and the nano-material is calcined at high temperature and cooled to room temperature under the protection of Ar / H2 to obtain N, P double-doped graphitize carbon material. The phenylhydroxyl metalloporphyrin containing the specific C-N conjugated macrocyclic structure is used as the assembly block,the phosphazene with the unique N, P structure is used as the precursor, acetonitrile with good solubility of phenylhydroxyl metalloporphyrin is used as a solvent, and porphyrin-phosphazene composition is realized by self-assembly polymerization. By adjusting the molar ratio of TPP to HCCP, the porphyrin-phosphazene self-assembled nanomaterial with good thermal stability and controllable morphology could be obtained. The graphitized carbon material with controllable N and P doping content and uniform distribution can be obtained by adjusting the carbonization temperature and heating rate, which has an important application in electrocatalytic oxygen reduction.

Description

technical field [0001] The invention belongs to the field of material chemistry and electrochemistry, and specifically relates to a N, P double-doped graphitized carbon material based on metalloporphyrin and phosphazene self-assembled nanomaterials, its preparation method and application. Background technique [0002] With energy consumption and serious environmental pollution, fuel cell vehicles with advantages such as high environmental protection, high conversion efficiency, short refueling time, and long mileage have entered people's daily life. Its large-scale use helps alleviate the huge demand for fossil energy, optimizes the structure of energy utilization, and promotes the sustainable development and progress of human beings to a certain extent. However, the reaction rate of the cathode oxygen reduction reaction (ORR) of the fuel cell is 6 to 7 orders of magnitude smaller than the reaction rate of the anode hydrogen oxidation reaction (HOR), which has greatly hinder...

Claims

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Application Information

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IPC IPC(8): H01M4/90H01M4/88B82Y30/00
CPCY02E60/50
Inventor 钟永任希彤白锋王静菡张文志刘双红
Owner HENAN UNIVERSITY
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