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A kind of sub-nanometer confinement novel Ru metal catalyst for hydrogenation and its preparation method and application

A metal catalyst and catalyst technology, applied in the energy field, can solve problems such as increasing costs, restricting production, application, and development, and achieve the effects of reducing usage, reducing catalyst costs, and simplifying the production process

Active Publication Date: 2022-06-24
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although noble metal catalysts have relatively good hydrogenation performance, the high loading of noble metal catalysts also greatly increases the cost, which has become a bottleneck restricting the large-scale production, application and development of organic liquid hydrogen storage technology.

Method used

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  • A kind of sub-nanometer confinement novel Ru metal catalyst for hydrogenation and its preparation method and application
  • A kind of sub-nanometer confinement novel Ru metal catalyst for hydrogenation and its preparation method and application
  • A kind of sub-nanometer confinement novel Ru metal catalyst for hydrogenation and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Weigh 0.145g of ruthenium acetate (Ru wt%=40-45, Mw=732.52) and 0.357g of o-phenanthroline monohydrate (C 12 H 8 N 2 ·H 2 O, Mw=198.22g / mol, molar ratio=1:3.03) was placed in a round-bottomed flask, 40ml of absolute ethanol was added, the oil bath in the fume hood was heated to reflux at 100°C for 90min, the round-bottomed flask was taken out, and the solvent was transferred to 100ml beaker. Weigh 6.000 g of silicon dioxide, add it to a beaker, stir evenly with a spatula, and the solid is in the shape of purple-red mud. The uniformly stirred solid was dried in an oven at 70° C. (overnight) for 8 h to obtain a yellow powder precursor. Put an appropriate amount of yellow powder in a tube furnace, pass 10% Ar / H 2 (H 2 The volume content is 10%) mixed gas, reduced at 1000 ° C for 4 h, and a new Ru catalyst was obtained. The physical adsorption and desorption curve and pore size distribution of the catalyst are as follows: figure 1 shown, from figure 1 It can be seen...

Embodiment 2

[0045] An appropriate amount of the catalyst precursor powder in Example 1 was taken out, placed in a tube furnace, and fed with 10% Ar / H 2 (H 2 volume content of 10%) mixed gas, reduced at 1000 ° C for 4 h, to obtain a new type of Ru catalyst. The hydrogenation experiment of organic liquid hydrogen storage material was carried out using 0.2 g of this catalyst. Wherein the selected hydrogen storage material is 2.0g nitroxylcarbazole, 40ml of cyclohexane is added as a solvent, the reaction pressure is 7MPa, the reaction temperature is 140°C, the rotation speed is 10rev / s, and the reaction time is 45min to realize azopropylcarbazole All azoles are hydrogenated without other by-products. The hydrogenation reaction rate of this new catalyst to nitrocarbazole is as follows image 3 shown.

Embodiment 3

[0047] An appropriate amount of the catalyst precursor powder in Example 1 was taken out, placed in a tube furnace, and fed with 10% Ar / H 2 (H 2 volume content of 10%) mixed gas, reduced at 1000 ° C for 4 h, to obtain a new type of Ru catalyst. 0.2g of this catalyst was used to carry out the cyclic hydrogenation experiment of organic liquid hydrogen storage material (nitropropylcarbazole). In each hydrogenation performance test, 2.0g of nitropropylcarbazole was selected as the hydrogen storage material, 40ml of cyclohexane was added as a solvent, the reaction pressure was 7MPa, the reaction temperature was 140°C, and the rotational speed was 10rev / s. Hydrogenation data results such as Figure 4 shown. from Figure 4 It can be seen from the above that the hydrogenation performance of the five-cycle hydrogenation experiments has gradually decreased, but the complete hydrogenation can be basically achieved within 90 min, indicating that the catalyst can be recycled for many t...

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Abstract

The invention discloses a novel subnano-confined Ru metal catalyst for hydrogenation of an organic liquid hydrogen storage material, a preparation method and application thereof, and belongs to the field of energy. The pore volume of the catalyst is 0.7-1.1cm 3 / g, the specific surface area is 400‑1000m 2 / g, the Ru metal loading in the catalyst is 0.05-0.7%, and the Ru metal particle size is between 0.2-2nm. The method uses silica / alumina / titanium dioxide / carbon black as the carrier, metal Ru is loaded on the carrier by the method of organometallic complexation, and then the catalyst is obtained through the process of high-temperature calcination and reduction, which can greatly reduce the precious metal Ru. dosage, while not reducing or even accelerating the hydrogenation reaction rate of organic liquid hydrogen storage materials. The catalyst has good cycle performance and can be used repeatedly without losing activity. The catalyst can be applied to the hydrogenation reaction of organic liquid hydrogen storage materials, especially carbazole hydrogen storage materials.

Description

technical field [0001] The invention belongs to the field of energy, and in particular relates to a new sub-nanometer confinement Ru metal catalyst for hydrogenation of organic liquid hydrogen storage materials and a preparation method and application thereof. Background technique [0002] Hydrogen energy is an important energy related to the future development of the world, and hydrogen storage technology is a key factor restricting the large-scale use of hydrogen energy. Compared with traditional hydrogen storage methods, organic liquid hydrogen storage technology has attracted social attention due to its high hydrogen storage density, stability at room temperature and ambient pressure, low cost, and easy transportation. In the process of addition and dehydrogenation of organic liquid hydrogen storage materials, the commonly used Ru catalyst is expensive, which increases the technical cost. Therefore, it is very important to find a more efficient and inexpensive catalyst....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/46B01J35/02B01J35/10C01B3/00
CPCY02E60/32
Inventor 杨明李根董媛
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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