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Preparation method of dual-activity monatomic ammonia synthesis catalyst

A catalyst and dual-activity technology, which is applied in the field of preparation of dual-activity single-atom ammonia synthesis catalysts, to achieve the effects of economical and easy-to-obtain raw materials, stable product performance, and convenient methods

Inactive Publication Date: 2018-08-24
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, during the course of this great invention, unprecedented difficulties were encountered

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  • Preparation method of dual-activity monatomic ammonia synthesis catalyst
  • Preparation method of dual-activity monatomic ammonia synthesis catalyst
  • Preparation method of dual-activity monatomic ammonia synthesis catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] 1) Weigh 4.04gFe(NO 3 ) 3 9H 2 O and 2.38 g CoCl 2 ·6H 2 O, measure 25mL of absolute ethanol in a 50mL beaker ①, stir until dissolved. Take 73mL TEOS and 6.5mL HCl solution into a 200ml beaker ②, the water-to-silicon ratio is about 3, stir evenly; add 2.40g urea into the beaker ②, stir to fully dissolve the urea. Pour the solution in beaker ① into beaker ②, and stir to make it evenly mixed. Pour the mixed solution into a 250mL round bottom flask, adjust the pH of the system to 4.5, heat, stir and reflux at 80-90°C for 2 hours, and place the slightly cooled flask in an incubator at 40°C for 1 day to obtain the initial condensation. glue. The obtained product in the gel state was further vacuum-dried at 60° C. for 1 day to obtain a solid gel.

[0047] 2) Put the product obtained in the above steps into a tube furnace for high-temperature calcination under nitrogen protection at a heating rate of 5°C / min and temperature control at 700°C. After calcination for 8 hour...

Embodiment 2

[0051] 1) Weigh 4.06gFe(NO 3 ) 3 9H 2 O and 2.50 g CuSO 4 ·5H 2 O, measure 25mL of absolute ethanol in a 50ml beaker ①, stir until dissolved. Take 76mL TEOS and 6.8mL HCl solution into a 200ml beaker ②, the water-to-silicon ratio is about 5, stir evenly; add 2.43g urea into the beaker ②, stir to fully dissolve the urea. Pour the solution in beaker ① into beaker ②, and stir to make it evenly mixed. Pour the mixed solution into a 250mL round bottom flask, adjust the pH of the system to 4.0, heat, stir and reflux at 80-90°C for 2 hours, and place the slightly cooled flask in an incubator at 40°C for 1 day to obtain the initial condensation. glue. The obtained product in the gel state was further vacuum-dried at 60° C. for 1 day to obtain a solid gel.

[0052] 2) Put the product obtained in the above steps into a tube furnace for high-temperature calcination under nitrogen protection at a heating rate of 10° C. / min and temperature control at 600° C. After 8 hours of calcina...

Embodiment 3

[0055] 1) Weigh 4.12gFe(NO 3 ) 3 9H 2 O and 2.63g NiSO 4 ·6H 2 O, measure 25mL of absolute ethanol in a 50mL beaker ①, stir until dissolved. Take 50mL TEOS and 6.8mL HCl solution into a 200ml beaker ②, the water-to-silicon ratio is about 15, stir evenly; add 2.5g urea into the beaker ②, stir to fully dissolve the urea. Pour the solution in beaker ① into beaker ②, and stir to make it evenly mixed. Pour the mixed solution into a 250ml round bottom flask, adjust the pH of the system to 5.0, heat, stir and reflux at 80-90°C for 2 hours, place the slightly cooled flask in an incubator at 40°C for 1 day to obtain the initial condensation glue. The obtained product in the gel state was further vacuum-dried at 60° C. for 1 day to obtain a solid gel.

[0056] 2) Put the product obtained in the above steps into a tube furnace for high-temperature calcination under nitrogen protection at a heating rate of 5°C / min, controlled at 600°C, and calcine for 6 hours to obtain a black soli...

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Abstract

The invention discloses a preparation method of a dual-activity monatomic ammonia synthesis catalyst. Ferric iron salt and divalent transition metal salt serve as raw materials, bimetal containing gelis prepared by a sol-gel method and calcined in inert gas atmosphere to obtain a black solid product, and then the black solid product is reduced by a reducing agent to obtain the dual-activity monatomic ammonia synthesis catalyst. In the sol-gel method, alcohols solvents and urea serve as coagulant aids, and tetraethyl orthosilicate is hydrolyzed under acid catalysis to prepare the bimetal containing gel. The raw materials are economical and easy to obtain, the method is convenient, product performances are stable, recycling is facilitated, and the catalyst can be used for synthesizing ammonia at room temperature and under normal pressure.

Description

technical field [0001] The invention relates to a preparation method of a dual-activity single-atom ammonia synthesis catalyst, which belongs to the technical field of chemical engineering industrial catalysis. Background technique [0002] The nitrogen cycle is one of the most important cycles in nature to maintain life activities on the earth. It has always been a dream of scientific and technological workers to directly reduce nitrogen in the air to ammonia under normal temperature and pressure conditions like nitrogen-fixing microorganisms in nature. On September 9, 1913, the world's first Haber-Bosch ammonia synthesis plant was completed and put into operation in Oppau, Germany, with a daily output of 30 tons of ammonia. This is an epoch-making monument for human beings to conquer nature. The great success of the synthetic ammonia industry has changed the history of world food production. However, during the course of this great invention, unprecedented difficulties we...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/75B01J23/745B01J23/755B01J37/03B01J37/08B01J37/16C01C1/02
CPCC01C1/02B01J23/745B01J23/75B01J23/755B01J37/036B01J37/082B01J37/16B01J35/393B01J35/23B01J35/33Y02P20/52
Inventor 张其坤娄文雪王艺谋周升阳刘宝良
Owner SHANDONG NORMAL UNIV
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