A kind of nano ruthenium carbon catalyst and its preparation method and application

A carbon catalyst and nano-ruthenium technology, which is applied in the field of high-selectivity and high-stability nano-ruthenium carbon catalyst and its preparation, can solve the problems of low catalytic selectivity and stability, avoid desorption and migration, reduce industrial waste, and reduce reaction mild effects

Active Publication Date: 2021-05-28
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The main purpose of the present invention is to provide a nano ruthenium carbon catalyst with high catalytic selectivity and stability and its preparation method, to overcome the catalytic selection of existing Ru-based catalysts for the hydrogenation of aromatic ring compounds to prepare cyclohexyl derivatives Disadvantages such as low sex and stability

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  • A kind of nano ruthenium carbon catalyst and its preparation method and application
  • A kind of nano ruthenium carbon catalyst and its preparation method and application
  • A kind of nano ruthenium carbon catalyst and its preparation method and application

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[0023] One aspect of the embodiments of the present invention provides a method for preparing a nano-ruthenium carbon catalyst, which is prepared by stepwise deposition and precipitation combined with staged roasting, specifically including:

[0024] Provide activated carbon as a carrier;

[0025] Immersing the activated carbon in an aqueous ruthenium salt solution, adding a basic compound, stirring and standing, filtering, drying and roasting to obtain the first ruthenium carbon precursor;

[0026] Immersing the first ruthenium-carbon precursor in an auxiliary aqueous solution, adding a basic compound, stirring and standing, filtering, and then drying to obtain a second ruthenium-carbon precursor;

[0027] In a protective atmosphere, the second ruthenium carbon precursor is subjected to segmental roasting treatment to obtain the third ruthenium carbon precursor;

[0028] The third ruthenium carbon precursor is reduced to obtain a nanometer ruthenium carbon catalyst.

[0029...

Embodiment 1

[0071] Weigh 50.00 g of pretreated activated carbon, add it to 300 mL of aqueous solution containing 5.56 g of ruthenium trichloride hydrate and stir for 3.0 h, then use 1.0 mol L -1 Adjust the pH of the mixed slurry to 9.0 with aqueous sodium hydroxide solution, continue to stir for 4.0 h, let it stand for 2.0 h, filter, wash the filter cake with water until it is neutral and free of chloride ions, and then dry it at 100°C for 4.0 h. 2 Calcined at 250° C. for 3.0 h under atmosphere, then added to an aqueous solution containing 4.84 g of zinc nitrate hexahydrate and continued to stir for 2.0 h. The pH adjustment and drying process were the same as above. in N 2 In the atmosphere, it was fired at 150°C for 4.0h, then at 400°C for 4.0h, and finally in H 2 :N 2 = 1:9 (v / v) reduction at 200° C. for 3.0 h in an atmosphere to obtain a nano-ruthenium carbon catalyst with a dispersion of 79.5%, a ruthenium loading of 4.0%, and a zinc loading of 2.0%. The HADDF-STEM figure of the ob...

Embodiment 2

[0073] Weigh 50.00 g of pretreated activated carbon, add it to 300 mL of aqueous solution containing 6.10 g of ruthenium acetylacetonate and stir for 0.5 h, then use 1.0 mol L -1 Adjust the pH of the mixed slurry to 12.0 with sodium carbonate aqueous solution, continue to stir for 1.0 h, let it stand for 2.0 h, filter, wash the filter cake with water until it is neutral and free of chloride ions, then dry it at 120 ° C for 4.0 h, and then dry it under N 2 Calcined at 400°C for 4.0 hours under atmosphere, then added to an aqueous solution containing 4.00 g of copper nitrate trihydrate and continued to stir for 4.0 hours, and the pH adjustment and drying process were the same as above. in N 2 In the atmosphere, first bake at 300°C for 2.0h, then at 600°C for 2.0h, and finally in H 2 :N 2 =3:7 (v / v) reduction at 120° C. for 10.0 h in an atmosphere to obtain a nano-ruthenium carbon catalyst with a dispersion of 72.2%, a ruthenium loading of 3.0%, and a copper loading of 2.0%.

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Abstract

The invention discloses a nano-ruthenium carbon catalyst as well as a preparation method and application thereof. The catalyst includes active carbon, active ruthenium particles supported thereon and auxiliary components, and the auxiliary components include zinc, copper, nickel and the like. The preparation method comprises: immersing activated carbon in an aqueous solution of ruthenium salt, adding a basic compound, stirring and standing still, filtering and drying, and roasting to obtain the first ruthenium carbon precursor, then immersing in an aqueous solution of an auxiliary agent, and then adding a basic compound , after stirring and standing still, filter and dry to obtain the second ruthenium carbon precursor; in a protective atmosphere, the second ruthenium carbon precursor is subjected to segmental roasting treatment to obtain the third ruthenium carbon precursor, followed by reduction treatment, obtain the catalyst. The catalyst of the invention can be reused more than one hundred times in the hydrogenation reaction of aromatic ring compounds to prepare cyclohexyl derivatives, and has the advantages of long service life, low production cost, mild reaction conditions, high product purity and less industrial waste.

Description

technical field [0001] The invention relates to a nano-ruthenium carbon catalyst with high selectivity and high stability, a preparation method thereof, and its application in the reaction of preparing cyclohexyl derivatives by hydrogenation of aromatic ring compounds, belonging to the technical field of catalysts. Background technique [0002] Cyclohexyl derivatives are important synthetic intermediates or fine chemicals in the fields of petrochemical and fine chemicals. For example, cyclohexanediamine is an important raw material for the preparation of pharmaceutical intermediates and polyurethane; cyclohexanedicarboxylates are environmentally friendly It can be widely used in the fields of medical appliances, toys and food packaging; cyclohexylpropionic acid is an important organic synthesis intermediate, widely used in the production of pineapple esters, ferroelectric liquid crystal materials and farnesyl transferase inhibitors, etc. synthesis. Cyclohexyl derivatives ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/60B01J23/89B01J37/03B01J37/08B01J37/18C07C209/72C07C211/36
CPCB01J23/60B01J23/892B01J23/8926B01J37/035B01J37/08B01J37/18C07C209/72C07C2601/14C07C211/36
Inventor 丑凌军赵华华宋焕玲赵军杨建闫亮
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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