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A kind of efficient nitrogen reduction cobalt manganese oxide catalyst and preparation method thereof

A technology of cobalt manganese oxide and catalyst, which is applied in the field of high-efficiency nitrogen reduction cobalt manganese oxide catalyst and its preparation field, can solve the problems of low yield of synthetic ammonia, low Faradaic efficiency, etc., and achieves increased specific surface area, improved nitrogen reduction performance, The effect of increasing catalytic activity

Active Publication Date: 2022-05-17
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention overcomes the deficiencies in the prior art. The existing nitrogen reduction catalysts have the problems of low synthetic ammonia yield and low Faraday efficiency, and provides a high-efficiency nitrogen reduction cobalt-manganese oxide catalyst and its preparation method. From the perspective of cost, it improves the nitrogen reduction yield and Faradaic efficiency and maintains long-term stability

Method used

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  • A kind of efficient nitrogen reduction cobalt manganese oxide catalyst and preparation method thereof
  • A kind of efficient nitrogen reduction cobalt manganese oxide catalyst and preparation method thereof
  • A kind of efficient nitrogen reduction cobalt manganese oxide catalyst and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Step 1, take 9.7806g of pure aluminum (Al), 3.5516g of pure cobalt (Co), 1.6678g of pure manganese (Mn), a total of 12g samples, mix the 12g samples evenly, place them in an argon smelting furnace, and pump them down with a mechanical pump Vacuum to 1×10 -1 After Pa, turn off the mechanical pump and turn on the molecular pump to draw a high vacuum to 2.3×10 -3 Finally, the molecular pump is turned off, and the high-purity argon protective gas is introduced. The melting time of the raw material is 160s, and the front and back are smelted 5-6 times, so that the internal components of the alloy are fully mixed and evenly obtained. 80 co 13.3 mn 6.7 alloy ingot.

[0030] Step 2, after fully cooling, take out the alloy ingot and cut it into pieces, take 3g of it and clean it ultrasonically with absolute ethanol and dry it, then place it in a clean quartz tube, install it in a strip machine, and then vacuum it to 7.8 ×10 -3 After Pa, turn off the vacuum, adjust the coppe...

Embodiment 2

[0041] Step 1, according to the atomic percentage of pure aluminum is 80%, the atomic percentage of pure cobalt is 10%, and the atomic percentage of pure manganese is 10%. -1 After Pa, turn off the mechanical pump and turn on the molecular pump to draw a high vacuum to 2.0×10 -3 Finally, the molecular pump is turned off, and high-purity nitrogen protective gas is introduced. The melting time of the raw material is 240s, and the front and back are smelted 5-6 times, so that the internal components of the alloy are fully mixed and evenly obtained. 80 co 10 mn 10 alloy ingot.

[0042] Step 2, after cooling down sufficiently, take out the alloy ingot and cut it into pieces, take 3g of it and ultrasonically clean and dry it with anhydrous ethanol, place it in a clean quartz tube, install it in a strip machine, and then vacuumize it to 1 ×10 -2 After Pa, turn off the vacuum, adjust the copper roller speed to 2500 rpm, control the pressure difference between the quartz tube and t...

Embodiment 3

[0045] Step 1, according to the atomic percentage of pure aluminum is 70%, the atomic percentage of pure cobalt is 15%, and the atomic percentage of pure manganese is 15%, and the ingredients are placed in the argon melting furnace, and the mechanical pump is low vacuumed to 1×10 -1 After Pa, turn off the mechanical pump and turn on the molecular pump to pump a high vacuum to 3.0×10 -3 Finally, the molecular pump is turned off, and the high-purity helium protective gas is introduced. The melting time of the raw material is 120s, and the front and back are smelted 5-6 times, so that the internal components of the alloy are fully mixed and evenly obtained. 70 co 15 mn 15 alloy ingot.

[0046] Step 2, after cooling down sufficiently, take out the alloy ingot and cut it into pieces, take 3g of it and ultrasonically clean and dry it with anhydrous ethanol, place it in a clean quartz tube, install it in a strip machine, and then vacuumize it to 1 ×10 -2 After Pa, turn off the va...

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Abstract

The invention provides a high-efficiency nitrogen-reducing cobalt-manganese oxide catalyst and a preparation method thereof, according to the atomic percentage of pure aluminum being 70-80%, the atomic percentage of pure cobalt being 10-20%, and the atomic percentage of pure manganese being 10-20%. For batching, in an inert protective gas atmosphere, the batching is melted by an electric arc melting furnace to obtain an Al-Co-Mn alloy ingot, and the Al-Co-Mn alloy ingot is made into an Al-Co-Mn alloy strip through a strip machine, and the Al-Co-Mn alloy After the Co‑Mn alloy strip is placed in NaOH solution to remove Al in the Al‑Co‑Mn alloy strip, it is then placed in a tube furnace and raised to 280‑650 °C at a heating rate of 3‑9 °C / min After heat preservation for 1-5h, after natural cooling to room temperature 20-25°C, a cobalt-manganese oxide catalyst is obtained, wherein the cobalt-manganese oxide catalyst is composed of CoO and Mn 3 o 4 composition. From the perspective of cost saving, the catalyst improves the nitrogen reduction yield and Faradaic efficiency and maintains long-term stability.

Description

technical field [0001] The invention relates to the technical field of electrode catalytic materials, in particular to a high-efficiency nitrogen-reducing cobalt-manganese oxide catalyst and a preparation method thereof. Background technique [0002] NH 3 It plays a vital role in the earth's ecosystem, is widely used in industry and agriculture, and is also an alternative energy source for hydrogen storage. Before the 20th century, nitrogen reduction mainly came from nitrogenase in microorganisms. In 1950, Haber and Bosch invented a N 2 revert to The process requires high temperature (~700K) high pressure (~100atm) and H 2 Produced under such conditions, and will produce carbon dioxide leading to global warming. Therefore, at room temperature and pressure, the electrocatalytic conversion of N 2 reduced to NH 3 is very important. However, electrochemical nitrogen reduction (NRR) faces challenges such as breaking the stable N≡N and improving catalytic activity. [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/889C25B1/27C25B11/091
CPCB01J23/8892B01J23/002C25B1/00C25B11/091
Inventor 朱胜利肖琳崔振铎梁砚琴杨贤金
Owner TIANJIN UNIV
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