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A kind of preparation method of nano ruthenium carbon supported catalyst

A catalyst and carbon supported technology, applied in the field of catalysis, can solve the problems of low catalytic activity, easy loss of active components, low stability, etc., and achieve the effects of uniform particle size distribution, avoiding desorption and migration, and high dispersion.

Active Publication Date: 2018-08-28
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention aims at the disadvantages of low catalytic activity, low stability and easy loss of active components in existing catalysts used for hydrogenation of cinnamic acid to generate 3-cyclohexylpropionic acid, and provides a high-efficiency catalyst for hydrogenation of cinnamic acid. Preparation method of nano-ruthenium carbon-supported catalyst with catalytic activity and stability

Method used

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  • A kind of preparation method of nano ruthenium carbon supported catalyst
  • A kind of preparation method of nano ruthenium carbon supported catalyst
  • A kind of preparation method of nano ruthenium carbon supported catalyst

Examples

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Embodiment 1

[0022] Accurately weigh 50.00 g of pretreated activated carbon, add it into 300 mL aqueous solution containing 5.56 g ruthenium trichloride hydrate, stir and impregnate for 3 h, and then use 1.0 mol L -1 Adjust the pH of the mixed slurry to 9 with sodium carbonate aqueous solution, continue to stir for 4 h, let it stand for 2 h, filter, wash the filter cake with water until it is neutral and free of chloride ions, and then transfer it to an oven for 4 h at 100 ° C. 2 The atmosphere was first calcined at 150 °C for 4 h, then at 400 °C for 4 h, and finally in H 2 :N 2 =1:9 (v / v) atmosphere at 300 ° C for 3 h, that is, a highly dispersed nano-ruthenium carbon-supported catalyst with a ruthenium loading of 4.0% was obtained.

Embodiment 2

[0024] Accurately weigh 50.00 g of pretreated activated carbon, add it into 300 mL aqueous solution containing 4.13 g of ruthenium trichloride hydrate, stir and impregnate for 3 h, and then use 1.0 mol L -1 Sodium carbonate aqueous solution adjusted the pH of the mixed slurry to 9, continued to stir for 4 h, let it stand for 1 h, filtered, washed the filter cake with water until it was neutral and free of chloride ions, then transferred to an oven for 4 h at 100 °C, and dried under N 2 The atmosphere was first calcined at 150 °C for 4 h, then at 400 °C for 4 h, and finally in H 2 :N 2 =1:9 (v / v) reduction at 300°C for 3 h, and a highly dispersed nano-ruthenium carbon-supported catalyst with a ruthenium loading of 3.0% was obtained.

Embodiment 3

[0026] Accurately weigh 50.00 g of pretreated activated carbon, add it into 300 mL aqueous solution containing 7.02 g of ruthenium trichloride hydrate, stir and impregnate for 3 h, and then use 1.0 mol L -1 Sodium carbonate aqueous solution adjusted the pH of the mixed slurry to 9, continued to stir for 4 hours, stood still for 1 hour, filtered, washed the filter cake with water until it was neutral and free of chloride ions, and then transferred to an oven for drying at 100°C for 6 hours. N 2 The atmosphere was first calcined at 150 °C for 4 h, then at 400 °C for 2 h, and finally in H 2 :N 2 =3:7 (v / v) atmosphere at 120 ℃ for 10 h to obtain a highly dispersed nano-ruthenium carbon-supported catalyst with a ruthenium loading of 5.0%.

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Abstract

The invention discloses a method for preparing a nanometer ruthenium carbon-supported catalyst. The method includes the following steps: adding treated activated carbon to a ruthenium salt solution, stirring and impregnating it for 0.5-4 h, and then using an aqueous alkaline compound solution to adjust the activated carbon and ruthenium. The pH of the salt mixed slurry reaches 7-12, continue stirring for 1-6 hours, let it stand for 2-4 hours, and filter. After the filter cake is washed with water until neutral and free of chloride ions, the filter cake is heated at a temperature of 80-120°C. The treated ruthenium carbon precursor is obtained by drying for 4-12 hours under low temperature; the treated ruthenium carbon precursor is roasted in sections under inert atmosphere conditions; the roasted product is reduced to obtain highly dispersed nano-ruthenium carbon-loaded type Catalyst, the particle size of the ruthenium particles of the catalyst is 1‑4 nm. The method of the present invention has the advantages of low production cost, mild preparation conditions, less industrial waste, and long service life of the catalyst obtained.

Description

technical field [0001] The invention relates to a preparation method of a high-activity and high-stability nano-ruthenium carbon-supported catalyst used for hydrogenation of cinnamic acid to prepare 3-cyclohexylpropionic acid, belonging to the technical field of catalysis. Background technique [0002] 3-Cyclohexylpropionic acid, also known as pineapple acid, is an important intermediate in organic synthesis and pharmaceutical synthesis, and is widely used in the synthesis of spices, farnesyltransferase inhibitors and ferroelectric liquid crystal materials. It is mainly used in the industry to synthesize allyl cyclohexyl propionate (commonly known as pineapple ester). Pineapple ester is an additive with strong sweet pineapple fruit aroma, which is widely used in food, cosmetics and tobacco fields. The preparation methods of pineapple acid mainly contain benzaldehyde method and cyclohexanol method at present. The cyclohexanol method uses methyl acrylate and cyclohexanol as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/46B01J35/00C07C51/36C07C53/134
CPCC07C51/36B01J23/462B01J35/393C07C53/134
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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