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Nanometer nickel-based polyhedron catalyst used for aromatic ring hydrogenation, preparation method thereof and application thereof

A catalyst and polyhedron technology, which is applied in the field of nano-nickel-based polyhedron catalysts to achieve mild reaction conditions, improved hydrogenation activity and good stability

Inactive Publication Date: 2015-04-01
SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, currently, there are few reports on the catalytic hydrogenation of nickel nanoparticles exposed to different crystal faces.

Method used

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  • Nanometer nickel-based polyhedron catalyst used for aromatic ring hydrogenation, preparation method thereof and application thereof
  • Nanometer nickel-based polyhedron catalyst used for aromatic ring hydrogenation, preparation method thereof and application thereof
  • Nanometer nickel-based polyhedron catalyst used for aromatic ring hydrogenation, preparation method thereof and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Dissolve 0.003mol of nickel chloride and 0.036mol of sodium citrate [molar ratio 1:12] in 70mL of ethylene glycol, and stir to dissolve under heating at 45°C to obtain a uniform solution 1.

[0045] Then 0.006 mol of sodium hydroxide and 0.003 mol of benzoic acid [the molar ratio of the two is 2:1] were dissolved together in 15 mL of ethylene glycol, and the obtained solution was added dropwise to the above solution 1 to obtain solution 2.

[0046] Then, 0.018 mmol of sodium formate was weighed and dissolved in 15 mL of ethylene glycol to obtain solution 3.

[0047]Put solution 2 and solution 3 in a 90°C vacuum oven and dry for 30 minutes. After taking them out, quickly mix them (dried solution 2 and solution 3) in a 250mL three-necked bottle. Under the temperature of 220 ℃ of oil baths and accompanied by condensing and reflux, stirring and reacting for 18 hours, the product obtained was washed and separated with ethanol, and the reaction product was vacuum-dried at 75 ...

Embodiment 2

[0052] Dissolve 0.003mol of nickel nitrate and 0.03mol of potassium citrate [the molar ratio of the two is 1:10] in 70mL of ethylene glycol, stir and dissolve under heating at 45°C to obtain a uniform solution 1.

[0053] Then 0.027mol potassium hydroxide and 0.015mol benzoic acid [the molar ratio of the two is 9:5] were dissolved in 15mL of ethylene glycol, and the obtained solution was added dropwise to the above solution 1 to obtain solution 2.

[0054] Then, 0.036 mol of potassium formate was weighed and dissolved in 18 mL of ethylene glycol to obtain solution 3.

[0055] Dry solution 2 and solution 3 in a vacuum oven at 75°C for 50 minutes. After taking them out, quickly mix the two (dried solution 2 and solution 3) evenly in a 250mL three-neck bottle. Under a nitrogen atmosphere, condense and reflux reaction at 200°C oil bath temperature for 20 hours, wash and separate the obtained product with ethanol, and vacuum dry the reaction product at 90°C for 10 hours to obtain a...

Embodiment 3

[0058] Dissolve 0.003mol of nickel nitrate and 0.045mol of sodium citrate [the molar ratio of the two is 1:15] in 70mL of ethylene glycol, stir and dissolve under heating at 45°C to obtain a uniform solution 1.

[0059] Then 0.009 mol of sodium hydroxide and 0.006 mol of benzoic acid [the molar ratio of the two is 3:2] were dissolved together in 15 mL of ethylene glycol, and the obtained solution was added dropwise to the above solution 1 to obtain solution 2.

[0060] Then, 0.024 mol of sodium formate was weighed and dissolved in 15 mL of ethylene glycol to obtain solution 3.

[0061] Put solution 2 and solution 3 at 95°C for 35 minutes in vacuum, and after taking them out, quickly mix them (dried solution 2 and solution 3) evenly in a 250mL three-neck bottle. Under a nitrogen atmosphere, condense and reflux at a temperature of 215°C for 10 hours, wash and separate the obtained product with ethanol, and dry the reaction product in vacuum at 80°C for 16 hours to obtain a nanom...

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Abstract

The invention discloses a nanometer nickel-based polyhedron catalyst used for aromatic ring hydrogenation, a preparation method thereof and an application thereof. The catalyst is in a polyhedron structure and has a particle size of 2-100 nm. The catalyst is a single nanometer nickel polyhedron catalyst or a nanometer bimetal polyhedron catalyst (expressed as NiM). The preparation method comprises preparation of the nanometer nickel polyhedron catalyst or preparation of the nanometer bimetal polyhedron catalyst. The catalyst is applied to the catalytic aromatic ring hydrogenation. The catalyst has characteristics of stable structure, uniform shapes, appearances and dimensions, exposure of high-activity crystal faces, high reactivity for the aromatic ring hydrogenation, and the like. In addition, the catalyst has advantages of mild reaction conditions, good stability, easy separation of products from the catalyst, convenient recycle and reutilization, and the like. The catalyst has a good industrialization application prospect.

Description

technical field [0001] The invention relates to a catalyst, in particular to a nano-nickel-based polyhedron catalyst used for hydrogenation of aromatic rings and its preparation method and application. Background technique [0002] Cyclohexane is mainly used to produce cyclohexanol, cyclohexanone and adipic acid. The latter three are important raw materials for the manufacture of nylon-6 and nylon-66. Cyclohexane is also used as resin, grease, rubber and plasticizer and other solvents. The intermediate of cyclohexane, such as alkyl cyclohexanol, is industrially used to synthesize cyclohexanol soap with strong emulsifying ability and the first foaming agent and cleaning agent in the textile industry; cyclohexanedicarboxylic acid is rubber, Alternatives to ethylene glycol in paint and other industries. These cyclohexane intermediates are mainly produced by hydrogenation of aromatic rings, which are mainly divided into homogeneous catalytic hydrogenation and heterogeneous cat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/755B01J23/89B01J35/02B22F9/24C07C5/10C07C13/18C07C13/50
CPCY02P20/584
Inventor 孙予罕祝艳陈国祥
Owner SHANGHAI ADVANCED RES INST CHINESE ACADEMY OF SCI
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