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Catalyst for electrochemically synthesizing ammonia and preparing method thereof

A technology for synthesizing ammonia and catalysts, applied in physical/chemical process catalysts, chemical instruments and methods, organic compounds/hydrides/coordination complex catalysts, etc. The effect of reducing consumption and high catalytic efficiency

Active Publication Date: 2016-11-16
HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the expensive defects of noble metal catalysts in the prior art, and provide catalysts for electrochemical ammonia synthesis and preparation methods thereof

Method used

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  • Catalyst for electrochemically synthesizing ammonia and preparing method thereof
  • Catalyst for electrochemically synthesizing ammonia and preparing method thereof

Examples

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Embodiment 1

[0024] MOF(Cu) is selected as the metal-organic framework material, and the synthesis step is Cu(NO 3 ) 2 ·3H 2 O, 1,3,5-BTC, according to a certain molar ratio (Cu 2+ :1,3,5-BTC:H 2 O=3:6:2) were dissolved in 180ml of water and 180ml of absolute ethanol respectively, and after stirring for 1 hour until uniform, the Cu(NO 3 ) 2 ·3H 2 O solution was dropped into 1,3,5-BTC solution and stirred for 2 hours. The mixed solution was then transferred to a polytetrafluoroethylene-lined jelly, then loaded into a stainless steel hydrothermal jelly, and placed in an oven, kept at 120°C for 24 hours and then cooled to room temperature. The product was filtered and washed, and the final product was dried in a vacuum oven at 60°C to obtain a MOF (Cu) sample, whose XRD pattern is as follows figure 1 shown. With the mass ratio of MOF(Cu):graphite:nafion=80:15:5, where the concentration of nafion is 80wt%, mix it with absolute ethanol to make a slurry, and evenly coat it on 4cm 2 On h...

Embodiment 2

[0026] MOF(Cu) is selected as the metal-organic framework material, and the synthesis step is Cu(NO 3 ) 2 ·3H 2 O, 1,3,5-BTC, according to a certain molar ratio (Cu 2+ :1,3,5-BTC:H 2 O=3:6:2) were dissolved in 180ml of water and 180ml of absolute ethanol respectively, and after stirring for 1 hour until uniform, the Cu(NO 3 ) 2 ·3H 2 O solution was dropped into 1,3,5-BTC solution and stirred for 2 hours. The mixed solution was then transferred to a polytetrafluoroethylene-lined jelly, then loaded into a stainless steel hydrothermal jelly, and placed in an oven, kept at 120°C for 24 hours and then cooled to room temperature. The product was filtered and washed, and the final product was dried in a vacuum oven at 60°C to obtain a MOF (Cu) sample, whose XRD pattern is as follows figure 1 shown. With the mass ratio of MOF (Cu): acetylene black: polytetrafluoroethylene: = 85:13.5:1.5, wherein the concentration of polytetrafluoroethylene is 5wt%, mixed evenly with absolute e...

Embodiment 3

[0028] The metal-organic framework material is MOF(Fe), and the synthesis step is Fe(NO 3 ) 3 9H 2 O, 1,3,5-BTC, 5mol / LHF and water according to a certain molar ratio (Fe 3+ :1,3,5-BTC:HF:H 2 (0=1.0:0.66:2.0:280) were mixed and stirred for 3-4 hours. The mixture was then transferred to a polytetrafluoroethylene-lined box, loaded into a stainless steel hydrothermal box, placed in an oven, and reacted at 150 °C for 84 hours before cooling to room temperature. The product was filtered and washed, and the final product was dried in a vacuum oven at 60°C to obtain a MOF(Fe) sample, whose XRD pattern is as follows figure 1 shown. With the mass ratio of MOF(Fe):carbon black:nafion:=80:1:5, wherein the concentration of nafion is 90wt%, mixed with absolute ethanol to make a slurry, uniformly coated on 4cm 2 On hydrophobic carbon paper, dry at 100°C for 8h, used for electrochemical synthesis of ammonia experiment, the reaction temperature is 80°C, the voltage is -1.2V, the synthes...

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Abstract

The invention belongs to the field of electrosynthesis ammonia. A catalyst for electrochemically synthesizing ammonia is formed by coating a metal organic skeleton, auxiliary carbon and a binding agent on carbon paper. The catalyst has the advantages of being easy to prepare, low in cost and high in catalysis efficiency. By using the catalyst, ammonia can be synthesized at normal pressure and low temperature, and energy consumption is greatly reduced. Air can be directly used as a raw material for synthesizing ammonia, the raw material source is enriched, raw material cost is reduced, and synthesis ammonia cost is reduced.

Description

technical field [0001] The invention belongs to the field of electrochemical synthesis of ammonia, in particular to a catalyst for electrochemical synthesis of ammonia and a preparation method thereof. Background technique [0002] Ammonia is one of the chemical products with the largest output in the world. At present, the industry adopts the Haber method to synthesize ammonia. This method was invented by the German Haber in 1905. Ammonia synthesis by the Haber method uses hydrogen and nitrogen as raw materials, usually using iron as a catalyst, to synthesize ammonia under high pressure (20-50MPa) and high temperature (500°C). [0003] Electrochemical synthesis of ammonia breaks through the thermodynamic limitation of the traditional Haber method of ammonia synthesis. The reaction can be carried out at low temperature and normal pressure, which not only reduces the energy consumption required by the Haber method for high temperature and high pressure, but also reduces the r...

Claims

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Application Information

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IPC IPC(8): B01J31/22C25B1/00C25B11/04
CPCB01J31/1815B01J31/22B01J2531/16B01J2531/842B01J2531/845C25B1/00C25B11/075
Inventor 银凤翔何小波李国儒
Owner HANGZHOU INST OF ADVANCED MATERIAL BEIJING UNIV OF CHEM TECH
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