Silicon-based molecular sieve confinement oxygen reduction Me-N-C catalyst and preparation method thereof

A catalyst and molecular sieve technology, applied in the field of electrocatalysis, can solve the problems of easy decomposition and poor stability, and achieve the effect of strong catalytic activity and high stability

Pending Publication Date: 2021-08-24
CHONGQING UNIV OF ARTS & SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of catalyst has its own limitations, such as: poor stability, easy to decompose during heat treatment, etc.

Method used

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  • Silicon-based molecular sieve confinement oxygen reduction Me-N-C catalyst and preparation method thereof
  • Silicon-based molecular sieve confinement oxygen reduction Me-N-C catalyst and preparation method thereof
  • Silicon-based molecular sieve confinement oxygen reduction Me-N-C catalyst and preparation method thereof

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Experimental program
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preparation example Construction

[0038] The present invention also provides a preparation process for the catalyst, specifically comprising the following steps:

[0039] 1. According to the molar ratio of transition metal and TPTZ is 1:3, mix the transition metal and TPTZ evenly.

[0040] 2. Then add 20 mL of 0.2 mol / L HCl, dissolve and stir for 5 hours to form a complex. Then add molecular sieve (SiO 2 ), stirred at room temperature for 24 hours, allowing the complex to fully enter the aperture of the molecular sieve.

[0041] 3. Put the product obtained in step 2 into an oven, and raise the temperature of the oven step by step to 800-950°C under the protection of nitrogen (specifically: raise the temperature to the required temperature at a rate of 10°C / min), and then Keep warm for two hours. Then cool naturally to room temperature, take out the medicine, and obtain the required catalyst, grind and pack it into bags.

[0042] 4. The samples of each treatment group in step 3 are ultrasonically cleaned (3...

Embodiment 1

[0044] Embodiment one: prepare the catalyst of different transition metals

[0045] 1. Weigh 6 parts of tripyridine triazine (hereinafter referred to as: TPTZ), each 0.2g, as 6 treatments. The molecular formula of TPTZ is as follows:

[0046]

[0047] According to the molar ratio of added material and TPTZ is 1:3, add 5 kinds of different materials respectively in the TPTZ of each treatment; 2 Cl 2 ), treatment 2: 0.03631g copper chloride (CuCl 2 ), treatment 3: 0.05062g nickel chloride (NiCl 2 ), treatment 4: 0.04215g manganese chloride (MnCl 2 ), treatment 5: 0.02903g zinc chloride (ZnCl 2 ); leave another treatment as a blank group, treatment 6.

[0048] 2. Precursor preparation: Add 20 mL of 0.2 mol / L HCl to the above 6 groups of treatments, dissolve and stir for 5 hours to form a complex. Then add 0.2g of molecular sieve (SiO 2 ), stirred at room temperature for 24 hours, allowing the complex to fully enter the aperture of the molecular sieve.

[0049] 3. Put ...

Embodiment 2

[0051] Example 2: Performance testing and morphology characterization of different transition metal catalysts

[0052] 1. Electrochemical performance test.

[0053] (1) Weigh 1mg samples of Fe-C-N-900, Cu-C-N-900, NiC-N-900, Mn-C-N-900, and Zn-C-N-900 respectively, put them in 0.5mL sample tubes, and add 90μL distilled water and 10 μL of 0.5 mol / L naphthalene solution, and ultrasonically mix evenly to obtain a mixed solution. Use a pipette gun to pipette 10 μL of the mixed solution on the surface of the glassy carbon electrode, and place it to dry to obtain an electrode.

[0054] (2) After the electrode is dry, place the electrode in the 0.1mol / L KOH electrolyte solution prepared in advance, and oxygenate it for a period of time. Connect the circuit according to the correct circuit connection method, and then turn on the electrochemical workstation for electrochemical testing to detect the ORR catalytic activity of the sample.

[0055] And simultaneously prepare a series of p...

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Abstract

The invention belongs to the field of electro-catalysis, and particularly relates to a silicon-based molecular sieve confinement oxygen reduction Me-N-C catalyst and a preparation method thereof. The specific technical scheme is as follows: the oxygen reduction catalyst is prepared by adding a transition metal into TPTZ to form a complex, then adding a molecular sieve, and limiting and wrapping the complex by the molecular sieve. The invention provides a novel transition metal (M)-nitrogen doped carbon-based oxygen reduction catalyst. Transition metal (M) is added into tripyridine triazine (TPTZ), then a molecular sieve is added, a complex formed by the tripyridine triazine (TPTZ) and the transition metal M is drilled into the pore diameter of the molecular sieve to be wrapped, then heat treatment is conducted, and the needed transition metal-nitrogen-carbon electrocatalyst is formed. The catalyst has the advantages of high ORR catalytic activity and high stability, and is expected to become a substitute of a commercial Pt catalyst.

Description

technical field [0001] The invention belongs to the field of electrocatalysis, and in particular relates to a silicon-based molecular sieve confined oxygen reduction Me-N-C catalyst and a preparation method thereof. Background technique [0002] The traditional cathode Pt catalyst has good catalytic activity for oxygen reduction (ORR), but Pt is a noble metal with scarce reserves and high price, which makes it difficult to promote and use in industry, which limits the rapid development of fuel cells. [0003] The prior art shows that nitrogen-doped carbon bases (such as graphene) have good ORR catalytic activity and are expected to replace Pt catalysts. However, this type of catalyst has its own limitations, such as poor stability and easy decomposition during heat treatment. [0004] Therefore, if a catalyst with strong ORR catalytic activity and good stability can be further provided on the basis of nitrogen-doped carbon-based catalysts, it is expected to promote the deve...

Claims

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Application Information

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IPC IPC(8): H01M4/90H01M4/88
CPCH01M4/9041H01M4/9083H01M4/8825H01M2004/8689Y02E60/50
Inventor 郭朝中刘瑶覃媛刘代军徐川岚欧子豪刘建平
Owner CHONGQING UNIV OF ARTS & SCI
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