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Preparation method of Ru-based catalyst with controllable particle size and application of Ru-based catalyst in'renewable energy electrolytic hydrogen production-ammonia synthesis'

A catalyst and ammonia synthesis technology, applied in the electrolysis process, electrolysis components, electrodes, etc., can solve the problem of low hydrogen pressure, and achieve the effects of easy molding, high-efficiency ammonia synthesis, and simple preparation method

Pending Publication Date: 2022-03-15
FUZHOU UNIV
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Problems solved by technology

However, for the development of this new reaction process, the main challenge is how to efficiently produce ammonia under relatively mild conditions, because the hydrogen pressure output from the water electrolysis process is low (<5 MPa) (Zheng J, Liao F, Wu S, et al. Efficient non-dissociative activation of dinitrogen toammonia over lithium-promoted ruthenium nanoparticles at low pressure. Angew. Chem. 2019, 131:17496–17502.)
However, the existing industrial ammonia synthesis catalysts are difficult to meet this synthesis condition, so the design and development of new and efficient ammonia synthesis catalysts has become the key point in the utilization of renewable energy-ammonia-hydrogen energy storage cycle route

Method used

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  • Preparation method of Ru-based catalyst with controllable particle size and application of Ru-based catalyst in'renewable energy electrolytic hydrogen production-ammonia synthesis'
  • Preparation method of Ru-based catalyst with controllable particle size and application of Ru-based catalyst in'renewable energy electrolytic hydrogen production-ammonia synthesis'
  • Preparation method of Ru-based catalyst with controllable particle size and application of Ru-based catalyst in'renewable energy electrolytic hydrogen production-ammonia synthesis'

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Experimental program
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Effect test

Embodiment 1

[0107] Disperse ruthenium trichloride (5.2mg, 0.025mmol), 1,10-phenanthroline (592mg, 3.0mmol), and melamine (900mg, 7.0mmol) in absolute ethanol (100mL), and after ultrasonic treatment for 10min, add Magnesium oxide (3.2 g, 0.08 mol) formed a homogeneous slurry; then sonicated for 10 min, then condensed and refluxed at 60 °C for 12 h, the solvent was removed by rotary evaporation at 60 °C, dried at 60 °C for 12 h and transferred to a tube furnace , under nitrogen atmosphere, at 2°C min -1 , heated up to 600°C, roasted for 2h, and after cooling down to room temperature, pour the obtained black powder into dilute nitric acid solution (1mol L -1 , 400mL), stirred at 80°C for 8h to remove magnesium oxide, then filtered and washed to neutral, then dried at 80°C for 12h to finally obtain Ru single-atom catalyst (marked as RuSAC), wherein the mass fraction of the active component was 0.39 wt%.

Embodiment 2

[0109] Triruthenium dodecacarbonyl (3.2mg, 0.005mmol), 1,10-phenanthroline (592mg, 3.0mmol) and melamine (900mg, 7.0mmol) were dispersed in absolute ethanol (100mL), and after ultrasonic treatment for 10min, Add magnesium oxide (6.4 g, 0.16 mol) to form a homogeneous slurry; then sonicate for 10 min, then reflux at 60 °C for 12 h, remove the solvent by rotary evaporation at 60 °C, and dry at 60 °C for 12 h before transferring to a tube furnace In nitrogen atmosphere, at 2°C min -1 , heated up to 600°C, roasted for 2h, and after cooling down to room temperature, pour the obtained black powder into dilute nitric acid solution (1mol L -1 , 400mL), stirred at 80°C for 8h to remove magnesium oxide, then filtered and washed to neutral, and dried at 80°C for 12h to finally obtain Ru cluster catalysts (marked as RuACCs), wherein the mass fraction of the active component was 0.40 wt%.

Embodiment 3

[0111] Triruthenium dodecacarbonyl (14.2mg, 0.022mmol) and 1,10-phenanthroline (298mg, 1.5mmol) were dispersed in a mixed solution of absolute ethanol and tetrahydrofuran (50mL, V / V=1:1), ultrasonic After processing for 10 min, magnesium oxide (6.4 g, 0.16 mol) was added to form a homogeneous slurry; then ultrasonic treatment was performed for 10 min, and then condensed and refluxed in a microwave single-mode reactor at 60 ° C for 12 h, the solvent was removed by rotary evaporation at 60 ° C, and the After drying at 60°C for 12h, transfer to a tube furnace, under nitrogen atmosphere, at 2°C min -1 , heated up to 600°C, roasted for 2h, and after cooling down to room temperature, pour the obtained black powder into dilute nitric acid solution (1mol L -1 , 200mL), stirred at 80°C for 8h to remove magnesium oxide, then filtered and washed to neutral, and dried at 80°C for 12h to finally obtain Ru subnano-cluster catalysts (marked as Ru SNCs), wherein the mass of the active compone...

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Abstract

The invention provides a preparation method of a Ru-based catalyst and application of the Ru-based catalyst in renewable energy electrolysis hydrogen production-ammonia synthesis, and the method specifically comprises the following steps: (1) uniformly dispersing a nitrogen-containing organic matter and magnesium oxide in a solvent to prepare slurry; (2) heating and roasting the slurry in the step (1) to obtain a roasted product; and (3) treating the roasted product in an acid solution to remove magnesium oxide to obtain the Ru-based catalyst, wherein the ruthenium precursor and the nitrogen-containing organic matter can be dispersed in the solvent in the step (1), or the ruthenium precursor can be added after roasting is finished, and the Ru-based catalyst is prepared. In the Ru-based catalyst, Ru exists in different scale forms, the ammonia synthesis performance of the Ru-based catalyst at low temperature can be adjusted by adjusting the particle size of Ru, and efficient ammonia synthesis under mild conditions is achieved.

Description

technical field [0001] The invention relates to the field of preparation of catalyst materials, in particular to a Ru-based catalyst with controllable particle size, a preparation method thereof, and its performance research application in "renewable energy electrolytic hydrogen production-synthetic ammonia". Background technique [0002] Hydrogen energy is an ideal clean energy and one of the feasible solutions to the fossil energy crisis. Hydrogen energy storage can use renewable energy to electrolyze water to produce hydrogen, which can be converted into stable chemical energy hydrogen, and the stored hydrogen can be converted into electrical energy through internal combustion engines, fuel cells, etc., to realize the storage-release energy cycle of renewable energy. The recycling of hydrogen energy is suitable for large-scale application. However, there are still key problems to be solved in the large-scale promotion and application of hydrogen energy, namely the storag...

Claims

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Application Information

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IPC IPC(8): C25B11/093C25B1/04C25B1/27
CPCC25B11/093C25B1/04C25B1/27Y02P20/133
Inventor 王秀云罗宇江莉龙
Owner FUZHOU UNIV
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