Preparation method of defect-rich Mn-Co metal oxide catalyst

An oxide, defect-rich technology, used in metal/metal oxide/metal hydroxide catalysts, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve problems such as unfavorable active site exposure, hard agglomeration, etc. Achieve the effect of inhibiting metal ion agglomeration and refining metal ion dispersion

Pending Publication Date: 2022-05-03
CHONGQING JIAOTONG UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, small-sized particles with high surface energy will inevitably undergo hard agglomeration during heat treatment, which is not conducive to the exposure of active sites.

Method used

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  • Preparation method of defect-rich Mn-Co metal oxide catalyst
  • Preparation method of defect-rich Mn-Co metal oxide catalyst
  • Preparation method of defect-rich Mn-Co metal oxide catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 0.1g Mn(NO 3 ) 2 4H 2 O, 0.47g Co(NO 3 ) 2 ·6H 2 O, 0.420g of 1,3,5-benzenetricarboxylic acid was mixed and placed in a ball mill jar. Dissolve 160 μL of formic acid in 1 mL of N,N-dimethylformamide, then transfer the solution to a ball mill, mix it with solid powder to obtain a suspension, add 420 μL of triethylamine for deprotonation treatment. Tighten the ball mill jar, and fix it in the slot of the vibratory high-energy ball mill, and the milling reaction time is 30 minutes. Centrifuge the product with N,N-dimethylformamide and absolute ethanol and filter, and dry the remaining solid powder in a drying oven at 60°C for 2 hours, and calcinate in a muffle furnace to obtain the target Mn-Co metal oxide catalyst (A), the sample BET specific surface area is 62.8m 2 g -1 . The calcination atmosphere is air, the calcination temperature is 400°C, the heating rate of the muffle furnace is 4°C / min, and the holding time is 2 hours.

Embodiment 2

[0023] Take 0.2g Mn(NO 3 ) 2 4H 2 O, 0.35g Co(NO 3 ) 2 ·6H 2 O, 0.420g of 1,3,5-benzenetricarboxylic acid was mixed and placed in a ball mill jar. Dissolve 160 μL of formic acid in 1 mL of N,N-dimethylformamide, then transfer the solution to a ball mill, mix it with solid powder to obtain a suspension, add 420 μL of triethylamine for deprotonation treatment. Tighten the ball mill jar, and fix it in the slot of the vibratory high-energy ball mill, and the milling reaction time is 30 minutes. The product was centrifuged with N,N-dimethylformamide and absolute ethanol and filtered, and the remaining solid powder was dried in a drying oven at 60°C for 2 hours, and calcined in a muffle furnace to obtain the target Mn-Co metal oxide catalyst (B), the sample BET specific surface area is 72.3m 2 g -1 . The calcination atmosphere is air, the calcination temperature is 400°C, the heating rate of the muffle furnace is 4°C / min, and the holding time is 2 hours.

Embodiment 3

[0025] Take 0.3g Mn(NO 3 ) 2 4H 2 O, 0.23g Co(NO 3 ) 2 ·6H 2 O, 0.420g of 1,3,5-benzenetricarboxylic acid was mixed and placed in a ball mill jar. Dissolve 160 μL of formic acid in 1 mL of N,N-dimethylformamide, then transfer the solution to a ball mill, mix it with solid powder to obtain a suspension, add 420 μL of triethylamine for deprotonation treatment. Tighten the ball mill jar, and fix it in the slot of the vibratory high-energy ball mill, and the milling reaction time is 30 minutes. The product was centrifuged with N,N-dimethylformamide and absolute ethanol and filtered, and the remaining solid powder was dried in a drying oven at 60°C for 2 hours, and calcined in a muffle furnace to obtain the target Mn-Co metal oxide catalyst (C), the sample BET specific surface area is 85.8m 2 g -1 . The calcination atmosphere is air, the calcination temperature is 400°C, the heating rate of the muffle furnace is 4°C / min, and the holding time is 2 hours.

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Abstract

The invention discloses a preparation method of a defect-rich Mn-Co metal oxide catalyst, which comprises the following steps: synthesizing a Mn / Co bimetal MOFs precursor with coordination defects under the condition of high-energy ball milling, and then calcining to prepare a defect-rich Mn-Co metal oxide; by means of the characteristic that MOFs serving as a catalyst precursor can restrain metal ion agglomeration and the thought that a mechanochemical method constructs material defects, a Mn / Co bimetal MOFs precursor prepared through high-energy ball milling is calcined in air to form a defect-rich Mn-Co metal oxide catalyst, MOFs with a large number of coordination defects have a special structure which is ordered in a short range and disordered in a long range, and the defect-rich Mn-Co metal oxide catalyst is obtained. The method has the advantages that metal ions are dispersed, crystal grains are refined, feasibility is provided for preparing defect-rich Mn-Co metal oxides, the highest specific surface area of the prepared catalyst can reach 85.8 m < 2 > / g, and the proportion of surface defect oxygen accounts for about 60% of oxygen species.

Description

technical field [0001] The invention relates to the field of inorganic nanometer catalytic materials, in particular to a method for preparing a defect-rich Mn-Co metal oxide catalyst. Background technique [0002] Volatile organic compounds (Volatile organic compounds, VOCs) have become one of the main components of air pollutants, causing serious harm to the ecological environment and human health. Considering energy saving and environmental friendliness, low-temperature oxidation of light alkanes catalysts and process development is one of the research hotspots in industrial catalysis. Due to the high price of noble metal catalysts, its commercial application is limited, and in metal oxide catalysts, Mn-Co oxides with a spinel structure are one of the most effective active species for activating and cracking C-C bonds and C-H bonds. Catalytic elimination has great application potential. However, different preparation methods and post-synthetic modifications will affect t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/889B01J37/08B01J35/10C01G51/04B01D53/86B01D53/72B01D53/44
CPCB01J23/8892B01J23/002B01J37/086B01J37/0036B01J35/1014C01G51/04C01G51/40B01D53/8668B01D53/8687C01P2002/72C01P2002/85C01P2004/03C01P2006/12B01D2257/708
Inventor 李传强刘项王浩博彭涛柴倩倩李世民郭强
Owner CHONGQING JIAOTONG UNIVERSITY
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