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Hydrocarbons of carbon nano-tube loaded nickel-stannum and method of manufacturing the same and use thereof

A hydrogenation catalyst, carbon nanotube technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, preparation of organic compounds, etc., can solve problems such as limiting the conversion rate of nitrophenol

Inactive Publication Date: 2009-02-11
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

When the nitro group is reduced to an amine, a lot of adsorbed hydrogen will be consumed. If the activation of the adsorbed hydrogen atoms on the nickel is insufficient, the conversion rate of p-nitrophenol will be directly limited.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Put 50 grams of multi-walled carbon nanotubes into a round-bottomed flask filled with 100 milliliters of hydrochloric acid with a mass concentration of 25%, vibrate ultrasonically for 60 minutes, and let stand overnight. Then put the carbon nanotubes into 100 milliliters of nitric acid with a mass concentration of 32% and reflux for 10 hours, filter and dry for future use (carbon nanotubes with straight top openings and a diameter of about 10-15 nanometers). Then 24.63 grams of Ni(NO 3 ) 2 ·6H 2 O and 2.34 g Sn(NO 3 ) 2 2H 2 O was dissolved in water and 20 g of the above carbon nanotubes were added, stirred for 12 hours and then filtered. Vacuum dried at 120°C overnight, then NO was removed under nitrogen protection at 450°C 3 - . The obtained substance is reduced by flowing hydrogen at 500 DEG C to prepare a carbon nanotube-supported nickel-tin hydrogenation catalyst.

[0029] 280 gram of water are dropped into 500 milliliters of reduction reactors with stirri...

Embodiment 2

[0032] Put 60 grams of multi-walled carbon nanotubes into a round-bottomed flask filled with 100 milliliters of 30% hydrochloric acid, vibrate ultrasonically for 40 minutes, and let stand overnight. Then put the carbon nanotubes into 100 milliliters of nitric acid with a mass concentration of 40% to reflux for 5 hours, filter and dry for later use (carbon nanotubes with curved top openings and a diameter of about 10-15 nanometers). Then 24.63 grams of Ni(NO 3 ) 2 ·6H 2 O and 5.85 g Sn(NO 3 ) 2 2H 2 O was dissolved in water and 30 g of carbon nanotubes were added, stirred for 15 hours and then filtered. Vacuum dried at 125°C overnight, then NO was removed under nitrogen protection at 440°C 3 - . Reducing the obtained substance by flowing hydrogen at 505° C. to prepare a carbon nanotube-supported nickel-tin hydrogenation catalyst.

[0033] Operation process is with embodiment 1. 120 grams of p-nitrophenol (purity is 95%), 280 grams of solvent ethanol, 12 grams of catal...

Embodiment 3

[0035] Put 50 grams of multi-walled carbon nanotubes into a round-bottomed flask filled with 100 milliliters of 20% hydrochloric acid, vibrate ultrasonically for 50 minutes, and let stand overnight. Then put the carbon nanotubes into 100 ml of nitric acid with a mass concentration of 30% to reflux for 4 hours, filter and dry for later use (carbon nanotubes with straight top openings and a diameter of about 10-15 nanometers). Add 19.70 g of Ni(NO 3 ) 2 ·6H 2 O and 2.34 g Sn(NO 3 ) 2 2H 2 O was dissolved in water and the above 22.50 g of carbon nanotubes were added, stirred for 24 hours and then filtered. Vacuum dried at 110°C overnight, then removed NO at 455°C under nitrogen protection 3 - . The obtained substance is reduced by flowing hydrogen at 490° C. to prepare a carbon nanotube-loaded nickel-tin hydrogenation catalyst.

[0036] Operation process is with embodiment 1. 100 grams of p-nitrophenol (purity is 95%), 300 grams of solvent acetone, 8 grams of catalyst, ...

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Abstract

The invention relates to the technical field of fine chemical products, in particular to a hydrogeneration catalyst of carbon nanotube supported nickel-tin, and a preparation method and an application of the catalyst. The hydrogeneration catalyst essentially comprises nickel, tin and carbon nanotube, wherein, the mass ratio of the three substances is 5-10:1-5:20-80, and the nickel and the tin can be distributed on the surface and in the aperture gap of the carbon nanotube evenly. The catalyst can be used for the synthesis of paraaminophenol through the catalytic hydrogenation of paranitrophenol, the synthesizing process of paraaminophenol is of short flow, large production capability, low labor intensity, high yield, few equipment investment and low comprehensive cost, is environment friendly and energy saving, and realizes the continuous clean production of synthetic paraaminophenol.

Description

technical field [0001] The invention relates to the technical field of fine chemical products, in particular to a carbon nanotube-supported nickel-tin hydrogenation catalyst and its preparation method and application. Background of the invention [0002] Hydrogenation reduction of nitro compounds is an important unit reaction in chemical production. Platinum carbon and palladium carbon, commonly used non-supported catalysts for catalytic hydrogenation, are expensive, difficult to recycle, and easy to lose metal, which greatly affects the service life of the catalyst. The framework nickel has low cost, can be recycled and has no discharge of three wastes, and the conversion rate of reactants and the selectivity of products reach 93% and 98% respectively. [0003] Due to its small size, large specific surface area, and many surface active sites, nano-nickel powder has become a new type of high-efficiency catalyst, which has attracted great attention from researchers in the fi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/835B01J21/18C07C215/76C07C213/02
Inventor 刘必前汪前东李兰
Owner INST OF CHEM CHINESE ACAD OF SCI
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