Method for enhancing synthesis ammonia selectivity by ball-milling nitrogen-hydrogen mixed gas at normal temperature and normal pressure in water phase

A nitrogen-hydrogen mixing and ammonia synthesis technology, applied in the field of materials, can solve problems such as environmental pollution, large energy consumption, and high equipment requirements, and achieve the effects of improving selectivity, increasing sources and concentrations, and enhancing performance

Active Publication Date: 2021-04-13
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This process requires high equipment, consumes a lot of energy, and causes serious environmental pollution.

Method used

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  • Method for enhancing synthesis ammonia selectivity by ball-milling nitrogen-hydrogen mixed gas at normal temperature and normal pressure in water phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Put 50mL of pure water and 300g of stainless steel balls of different sizes in a stainless steel vacuum ball milling jar with a capacity of 250mL, and inject nitrogen-hydrogen mixture gas (10 vol% H 2 + 90vol%N 2 ) for 30 minutes, get rid of the air in the tank, seal the ball mill tank so that the tank is in an environment full of nitrogen-hydrogen mixture at normal temperature and pressure, and the volume of the mixture is 180mL;

[0020] (2) Install the ball mill jar prepared in step (1) in a planetary ball mill, mill at a rate of 600 rpm for 10 hours, and take out the ball mill jar after the reaction is completed;

[0021] (3) Take out the solution in the tank in step (2), let it stand still, take the supernatant, and centrifuge twice through the centrifuge to further remove the iron filings generated during the ball milling process, each time at 15000r / min, 5min;

[0022] (4) Detect the aqueous solution in step (3) by ion chromatography, and measure the NH in ...

Embodiment 2

[0025] (1) Put 50mL of pure water and 300g of stainless steel balls of different sizes in a stainless steel vacuum ball milling jar with a volume of 250mL, and inject a nitrogen-hydrogen mixture (5vol% H 2 + 95vol%N 2 ) for 30 minutes, get rid of the air in the tank, seal the ball mill tank so that the tank is in an environment full of nitrogen-hydrogen mixture at normal temperature and pressure, and the volume of the mixture is 180mL;

[0026] (2) Install the ball mill jar prepared in step (1) in a planetary ball mill, mill at a rate of 600 rpm for 10 hours, and take out the ball mill jar after the reaction is completed;

[0027] (3) Take out the solution in the tank in step (2), let it stand still, take the supernatant, and centrifuge twice through the centrifuge to further remove the iron filings generated during the ball milling process, each time at 14000r / min, 7min;

[0028] (4) Detect the aqueous solution in step (3) by ion chromatography, and measure the NH in the so...

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Abstract

The invention belongs to the technical field of materials, and particularly relates to a method for enhancing synthesis ammonia selectivity by ball-milling nitrogen-hydrogen mixed gas at normal temperature and normal pressure in a water phase. The method comprises the following steps: carrying out mechanochemical ball milling by using a planetary ball mill, putting stainless steel milling balls and pure water into a stainless steel ball milling tank, introducing nitrogen-hydrogen mixed gas with different volume ratios, carrying out direct ball milling at normal temperature and normal pressure, standing and centrifuging the solution after the reaction is finished, and verifying the existence of ammonium ions (NH4 +) in the solution by ion chromatography, and measuring the corresponding NH4 + concentration. Nitrogen and hydrogen mixed gas is introduced into water, so that the source and concentration of hydrogen protons required in the synthetic ammonia reaction are increased, the forward proceeding of the reaction is promoted, the selectivity of the mechanical ball-milling synthetic ammonia reaction is greatly improved, and the performance of the mechanical and chemical ball-milling synthetic ammonia reaction is enhanced. Meanwhile, water is used as a reactant, so that the abrasion between the grinding ball and the ball-milling tank body is relieved, and the service life of the ball-milling equipment is prolonged.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a method for mechanically ball-milling nitrogen-hydrogen mixed gas in water phase at normal temperature and pressure to enhance the reaction selectivity of synthetic ammonia. Background technique [0002] Ammonia (NH 3 ) plays a vital role in the fields of industry, agriculture, national defense, etc., and is an important raw material for synthetic fertilizers, fibers and explosives. Ammonia has a low liquefaction pressure (~8 atm) and high hydrogen density (17.8 wt%), which can serve as a potential hydrogen carrier. Ammonia synthesis is currently mainly carried out through the Haber-Bosch process, which requires high temperature (300-550°C), high pressure (15-25 MPa) conditions, and thermal catalysis under an iron-based catalyst. This process requires high equipment, consumes a lot of energy, and causes serious environmental pollution. Therefore, it is necessary...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01C1/04
CPCC01C1/04Y02P20/52
Inventor 何承溧崔晓莉陈阳邱栋陆雨瑄
Owner FUDAN UNIV
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