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A ruthenium-based ammonia synthesis catalyst with nitrogen-doped porous carbon material as carrier and preparation method thereof

A nitrogen-doped porous carbon, ruthenium-based catalyst technology, applied in chemical instruments and methods, ammonia preparation/separation, physical/chemical process catalysts, etc., can solve the problems to be further improved, high specific surface area, etc. Effects of specific surface area and strength, high specific surface area, and high ammonia synthesis activity

Active Publication Date: 2021-11-02
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN106513030A reports the introduction of melamine nitrogen-containing precursors on graphitized activated carbon, mechanical stirring and mixing, constant temperature water bath heating, and calcination to obtain nitrogen-doped activated carbon, but the nitrogen content obtained by this method is between 0.72-7.61wt%. between
Patent CN104785255A reports the introduction of nitrogen-containing precursors on commercial activated carbon, cooling after calcination, and Soxhlet extraction to obtain nitrogen-doped activated carbon with high specific surface area, but the nitrogen content obtained by this method is between 1-10wt%. When it is used as a carrier to prepare ruthenium catalyst, its ammonia synthesis performance needs to be further improved.
Patent CN107694594A reports a nitrogen-doped carbon material with immobilized metals obtained by mixing carbon materials with metal ion ammonia and carrying out microwave reaction in a carbon bath under an inert atmosphere, but the nitrogen content obtained by this method is between 1- 4wt%, and the specific surface area of ​​the prepared material is only 380~450m 2 / g
Obviously, the nitrogen-doped carbon materials prepared by the prior art are difficult to maintain high specific surface area and high nitrogen content at the same time, so they are not suitable as ideal support materials for ruthenium-based ammonia synthesis catalysts

Method used

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  • A ruthenium-based ammonia synthesis catalyst with nitrogen-doped porous carbon material as carrier and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 1) Dissolve 1.93 g zinc nitrate hexahydrate in 48 ml sodium hydroxide solution (6 mol / L);

[0029] 2) Dissolve 2.104 g of 2-methylimidazole in 9.6 ml of N,N-dimethylformamide (purity 99.5%), and then add 6.4 ml of sodium hydroxide (6 mol / L) solution;

[0030] 3) After mixing and stirring the solutions obtained in the above steps (1) and (2), they were heated and reacted in a hydrothermal kettle at a constant temperature of 120 °C for 4 hours to obtain a milky white solution, which was washed with methanol solution and centrifuged to obtain a solid product , and then dried at a constant temperature in a vacuum oven at 80°C for 12 hours to obtain a solid product;

[0031] 4) Put the solid product obtained in the above step (3) into a tube furnace, and in 10% (volume fraction) H 2 - Under the Ar atmosphere, the temperature was increased at a rate of 2 ℃ / min to 800 ℃ for 4 hours for high-temperature carbonization, and nitrogen-doped porous carbon materials were obtained; ...

Embodiment 2

[0035] 1) Dissolve 1.26 g zinc nitrate hexahydrate in 30 ml sodium hydroxide solution (6 mol / L);

[0036] 2) Dissolve 2.104 g of 2-methylimidazole in 15 ml of N,N-dimethylformamide (purity 99.5%), and then add 6 ml of sodium hydroxide (6 mol / L) solution;

[0037] 3) Mix and stir the solution obtained in the above steps (1) and (2) evenly, then heat and react at a constant temperature of 130 ℃ for 4 hours in a hydrothermal kettle to obtain a milky white solution, wash with methanol solution, and centrifuge to obtain a solid product , and then dried at a constant temperature in a vacuum oven at 70°C for 12 hours to obtain a solid product;

[0038] 4) Put the solid product obtained in the above step (3) into a tube furnace, and in 10% (volume fraction) H 2 - Under the Ar atmosphere, the temperature was raised to 700 °C at a heating rate of 2 °C / min for 5 hours for high-temperature carbonization, and nitrogen-doped porous carbon materials were obtained;

[0039]5) Dissolve 12.52...

Embodiment 3

[0042] 1) Dissolve 1.93 g zinc nitrate hexahydrate in 48 ml sodium hydroxide solution (6 mol / L);

[0043] 2) Dissolve 2.104 g of 2-methylimidazole in 9.6 ml of N,N-dimethylformamide (purity 99.5%), and then add 6.4 ml of sodium hydroxide (6 mol / L) solution;

[0044] 3) After mixing and stirring the solutions obtained in the above steps (1) and (2) evenly, heat and react in a hydrothermal kettle at a constant temperature of 140 °C for 4 hours to obtain a milky white solution, wash with methanol solution, and centrifuge to obtain a solid product , and then dried at a constant temperature in a vacuum oven at 80°C for 10 hours to obtain a solid product;

[0045] 4) Put the solid product obtained in the above step (3) into a tube furnace, in pure H 2 Nitrogen-doped porous carbon materials were obtained by heating at a rate of 2 °C / min to 900 °C for 3 hours in the atmosphere for high-temperature carbonization;

[0046] 5) Dissolve 12.52 ml of ruthenium nitrosyl nitrate solution (r...

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Abstract

The invention belongs to the technical field of fertilizer catalysts, and in particular relates to a ruthenium-based ammonia synthesis catalyst supported by a nitrogen-doped porous carbon material and a preparation method thereof. In the preparation process of the catalyst, first dissolve zinc nitrate hexahydrate in an alkaline aqueous solution, dissolve 2-methylimidazole in N, N-dimethylformamide, then add an alkaline aqueous solution, mix the above-mentioned solutions uniformly and heat reaction and carbonization to obtain a nitrogen-doped porous carbon material. dissolving chlorine-free ruthenium compound and polyvinylpyrrolidone together in ethylene glycol solution, heating, washing with ethanol-acetone mixed solution, and then adding ethanol solution; adding the above-mentioned porous carbon material and stirring, standing still, separating, drying and reducing to obtain the The ruthenium-based ammonia synthesis catalyst supported by nitrogen-doped porous carbon material not only has a higher specific surface area, but also has a higher nitrogen doping amount, so it has higher ammonia synthesis activity and has a better application prospect.

Description

technical field [0001] The invention belongs to the technical field of fertilizer catalysts, and in particular relates to a ruthenium-based ammonia synthesis catalyst supported by a nitrogen-doped porous carbon material and a preparation method thereof. Background technique [0002] The ammonia synthesis industry is a pillar industry of the national economy. The Haber-Bosch method currently used for industrial ammonia synthesis must produce ammonia under the harsh conditions of high temperature (400–500 °C) and high pressure (15–30 MPa), making the ammonia synthesis industry a high energy consumption and capital intensive industry. The key to saving energy and reducing consumption in the ammonia synthesis industry is the application of high-performance catalysts. Therefore, the research and design of high-efficiency ammonia synthesis catalysts has always been a research hotspot in the field of catalysis. At present, activated carbon-supported ruthenium catalysts are the most...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J35/10C01C1/04
CPCB01J27/24C01C1/0411B01J35/617Y02P20/52
Inventor 林炳裕上官志超倪军林建新江莉龙
Owner FUZHOU UNIV
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