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Preparation method of chloride-free activated carbon-loaded ruthenium-based ammonia synthesis catalyst

A technology for the synthesis of activated carbon and ammonia, which is applied in the direction of catalyst activation/preparation, ammonia preparation/separation, chemical instruments and methods, etc. It can solve the problems of ruthenium loss, safety risks, long washing time, etc., and achieves easy operation, reduced loss, highly active effect

Inactive Publication Date: 2018-08-24
FUZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, first loading ruthenium chloride on the carrier, and then washing with water to remove chloride ions, some ruthenium will be lost during the washing process. After loading and washing, the maximum loss of ruthenium may reach 10%, which is a huge loss for precious metals. waste, and the method of washing before loading is used, there is almost no loss of ruthenium in the catalyst preparation process, the economic benefit is remarkable, the activity and stability of the catalyst can also be stably controlled, and the quality of the catalyst product is more controllable; moreover, due to the The chloride ions on the surface of activated carbon and the hydroxyl, carboxyl and other groups on the surface of activated carbon have a strong bonding strength, which makes the washing time of the loaded chloride ions very long, and it is difficult to completely wash away the chloride ions, which leads to the use of chloride ions on the catalyst in industrial high-temperature and high-pressure equipment. pose a greater security risk

Method used

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  • Preparation method of chloride-free activated carbon-loaded ruthenium-based ammonia synthesis catalyst

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Embodiment 1

[0016] Take 0.1 mol / L RuCl 3 100 mL of aqueous solution, 50 mL of 0.6 mol / L KOH aqueous solution was added dropwise during stirring, and after mixing, let it stand for 1 h. Centrifuge the resulting mixture at 3000 r / min for 3 min. Pour out the supernatant. Then add absolute ethanol to stir, centrifuge and wash. The above washing process was repeated 5 times, and the ICP analysis of the washing solution showed that there was no ruthenium metal ion. Add 20 mL of HNO to the resulting precipitate 3 Solution (3 mol / L) to completely dissolve it, and then immerse it on activated carbon. The amount of ruthenium metal added based on the mass of activated carbon is 10%. The prepared sample was reduced in a nitrogen-hydrogen mixed atmosphere containing 75% hydrogen at 450°C for 6 hours, and then cooled to room temperature in the above atmosphere. Finally, the obtained sample is immersed in an aqueous potassium nitrate solution to a potassium metal content of 12% based on the mass of the ...

Embodiment 2

[0018] Divide 0.2 mol / LRuCl 3 50 mL of aqueous solution, 30 mL of 1.0 mol / L KOH aqueous solution was added dropwise during the stirring process, mixed and allowed to stand for 10 h, the resulting mixture was centrifuged at 3000 r / min for 3 min, and the supernatant was discarded. Then add absolute ethanol to stir, centrifuge and wash. The above washing process was repeated 15 times, and the ICP analysis of the washing liquid showed that there was no ruthenium metal ion. Add 80 mL of HNO to the resulting precipitate 3 Solution (1 mol / L) to completely dissolve it, and then immerse it on activated carbon. The amount of ruthenium metal added is 10% based on the mass of activated carbon. The prepared sample was reduced at 500°C for 4 hours in a 25% hydrogen-containing nitrogen-hydrogen mixed atmosphere, and cooled to room temperature in the above atmosphere. Finally, the obtained sample is immersed in an aqueous potassium nitrate solution until the amount of potassium metal is 12% b...

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Abstract

The invention relates to a preparation method of a chloride-free activated carbon-loaded ruthenium-based ammonia synthesis catalyst, and relates to a preparation method of a chloride-free ruthenium-based ammonia synthesis catalyst by using ruthenium chloride as a raw material and removing chloride ions. The preparation method specifically comprises the following steps of using the ruthenium chloride as the raw material, adding soluble alkaline, standing, settling, washing, and dissolving, so as to obtain a chloride-free ruthenium precursor; loading onto the activated carbon, and adding a KNO3(potassium nitrate) additive, so as to obtain the chloride-free activated carbon-loaded ruthenium-based ammonia synthesis catalyst. Compared with the ruthenium-based ammonia synthesis catalyst prepared the existing methods, the preparation method has the advantages that the ruthenium chloride is used as the raw material, the price is low, the preparation technology is simple, the operation is convenient, the chloride ions can be well removed, and the loss of noble metal, namely ruthenium, is reduced in the preparation process; the activity of the prepared catalyst is higher; the industrializedapplication prospect is better.

Description

Technical field [0001] The invention relates to a preparation technology of a ruthenium catalyst using nitrogen and hydrogen to synthesize ammonia in the synthetic ammonia industry in the chemical fertilizer field, and specifically relates to a preparation method of a chlorine-free activated carbon supported ruthenium-based ammonia synthesis catalyst. Background technique [0002] The synthetic ammonia industry occupies a pivotal position in the national economy. A large part of synthetic ammonia is used as nitrogen fertilizer, which promotes grain production. In addition, ammonia is also an indispensable and important raw material in many chemical production. Therefore, the invention and development of synthetic ammonia technology are of great significance to mankind. Currently, the commonly used ammonia synthesis catalyst precursors are divided into two types, chlorine-containing compounds and chlorine-free compounds. For example, hydrated ruthenium trichloride is a more comm...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J37/02B01J37/03B01J37/06B01J37/18C01C1/04
CPCB01J23/462B01J37/0213B01J37/031B01J37/06B01J37/18C01C1/0411Y02P20/52
Inventor 倪军刘瑞曹陈凤林炳裕林建新江莉龙
Owner FUZHOU UNIVERSITY
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