Self-supporting nanoporous nitrogen reducing catalyst and preparation method thereof

A nanoporous, self-supporting technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems such as limited stability, and achieve easy operation, simple process flow, and improved catalytic activity. Effect

Active Publication Date: 2019-11-12
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these catalysts have limited stability under strongly reducing conditions, and it is challenging to coat them efficiently on electrodes

Method used

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  • Self-supporting nanoporous nitrogen reducing catalyst and preparation method thereof
  • Self-supporting nanoporous nitrogen reducing catalyst and preparation method thereof
  • Self-supporting nanoporous nitrogen reducing catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Step 1, get pure iron (Fe) 4.8674g, pure iron triphosphorus (Fe 3 P) 3.4603g, pure molybdenum (Mo) 1.6723g, a total of 10g, 10g samples were mixed evenly, placed in an argon melting furnace, and vacuumed by a mechanical pump 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 4-5 times, so that the internal components of the alloy are fully mixed and evenly obtained to obtain Fe 80 Mo 10 P 10 alloy ingot.

[0027] Step 2, after cooling down sufficiently, take out the alloy ingot and cut it into pieces, take 3g and ultrasonically clean and dry it with anhydrous ethanol, place it in a clean quartz tube, install it in a belt spinner, and evacuate it to 7.8× 10 -3 After Pa, turn off the vacuum, adjust the speed of the copper roll...

Embodiment 2

[0036] Step 1, according to the mass percent of pure Fe 40%, the mass percent of pure Mo 10%, Fe 3 The mass percentage of P is 50% for batching, placed in the argon smelting furnace, and the mechanical pump is vacuumed to 1×10 -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 the high-purity argon protective gas is introduced. The melting time of the raw material is 120s, and the front and back are smelted 4-5 times, so that the internal components of the alloy are fully mixed and uniform, and the Fe-Mo-P alloy ingot is obtained.

[0037] Step 2, after fully cooling, take out the alloy ingot and cut it into pieces, take 3g and ultrasonically clean and dry it with absolute ethanol, place it in a clean quartz tube, install it in a belt spinner, and evacuate it to 7× 10 -5 After Pa, turn off the vacuum, adjust the speed of the copper roller to 1000 rpm, control the pressure ...

Embodiment 3

[0040] Step 1, according to the mass percent of pure Fe 60%, the mass percent of pure Mo 10%, Fe 3 The mass percentage of P is 30% for batching, placed in the argon smelting furnace, and the mechanical pump is 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, high-purity argon protective gas is introduced, the melting time of the raw material is 240s, and the front and back are smelted 4-5 times, so that the internal components of the alloy are fully mixed and uniform, and the Fe-Mo-P alloy ingot is obtained.

[0041] Step 2, after cooling down sufficiently, take out the alloy ingot and cut it into pieces, take 3g of it and ultrasonically clean it with absolute ethanol and blow it dry, put it in a clean quartz tube, install it in a belt spinner, and evacuate it to 8× 10 -5 After Pa, turn off the vacuum, adjust the speed of the copper roller to 3000 rpm, contr...

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Abstract

The invention provides a self-supporting nanoporous nitrogen reducing catalyst and a preparation method thereof. The preparation method comprises the following steps: batching, by mass, 40-60% of pureFe, 5-20% of pure Mo and 30-50% of Fe3P; in an inert protective gas atmosphere, melting the above ingredients with an electric arc melting furnace to obtain a Fe-Mo-P alloy ingot, and preparing a Fe-Mo-P alloy strip from the Fe-Mo-P alloy ingot by using a melt spinning machine; clamping and fixing the Fe-Mo-P alloy ingot with electrode holders, carrying out electrochemical de-alloying with phosphoric acid, wherein a reaction is carried out at a room temperature of 20-25 DEG C for 1,800-4,000 s, and then carrying out washing and drying to finally obtain the self-supporting nanoporous nitrogenreducing catalyst. The catalyst prepared in the invention has the characteristics of low cost, no toxicity and high chemical stability, and exhibits high electrocatalytic nitrogen reduction activity due to its high activity and electrical conductivity.

Description

technical field [0001] The invention relates to the field of electrochemical nitrogen reduction catalyst materials, in particular to a self-supporting nanoporous nitrogen reduction catalyst and a preparation method thereof. Background technique [0002] In the 1950s, people used the Haber-Bosch method to convert N 2 reduced to NH 3 , the process requires high temperature (~700K) high pressure (~100atm) and H 2 And so on, it will produce a lot of environmental pollution. Electrochemical nitrogen reduction can produce ammonia from air and water via renewable electricity. Therefore, at room temperature and pressure, the electrocatalytic conversion of N 2 reduced to NH 3 is very important. However, the electrochemical synthesis of ammonia still faces challenges such as breaking the stable N≡N and improving the catalytic activity. Noble metal-based materials are efficient NRR electrocatalysts, but are expensive and have limited availability, which hinders large-scale appli...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/19B01J35/10C25B11/06C25B11/03C25B1/00
CPCB01J27/19B01J35/1061B01J35/1066B01J35/1004B01J35/0033C25B11/03C25B1/00C25B11/091
Inventor 朱胜利肖琳崔振铎梁砚琴杨贤金
Owner TIANJIN UNIV
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