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Palladium/carbon nanotube catalyst and preparation and application thereof

A carbon nanotube and catalyst technology, which is applied in the palladium/carbon nanotube catalyst; field, achieves the effects of stable catalyst and simple and convenient operation

Inactive Publication Date: 2014-12-31
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, no catalysts that selectively support palladium nanoparticles inside or outside the lumen of carbon nanotubes have been used in heterogeneous asymmetric hydrogenation reactions.

Method used

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  • Palladium/carbon nanotube catalyst and preparation and application thereof
  • Palladium/carbon nanotube catalyst and preparation and application thereof
  • Palladium/carbon nanotube catalyst and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Weigh 12.0g of carbon nanotubes (average inner diameter 5-10nm, outer diameter 10-20nm) into a 1L round-bottomed flask, put in a magnetic stirrer, add 600mL concentrated nitric acid (mass concentration 65-68%), put on Reflux condenser, heat to 140°C with an oil bath, stir and reflux for 3 to 18 hours as needed, cool, filter, wash with deionized water until the pH value of the filtrate is neutral, put it in an oven at 80°C at a constant temperature of 24 to 48 hours, an open functionalized carbon nanotube support is obtained.

Embodiment 2

[0049] Preparation of palladium / carbon nanotube catalysts loaded with palladium nanoparticles inside the lumen of carbon tubes:

[0050] 1) In a round bottom flask, weigh palladium chloride (83.3 mg, palladium content ≥ 60%, 5% palladium loading), add 25 mL of acetone, and then add 30 μL of concentrated hydrochloric acid with a mass fraction of 37% to help dissolve chlorine Palladium, shake for a few minutes to dissolve the palladium chloride, stir evenly, then add 1.0g of dry functionalized carbon nanotube support (average inner diameter 5-10nm, outer diameter 10-20nm), electromagnetically stir to mix evenly, and then place In an ultrasonic oscillator, turn on the sonication for 3 hours.

[0051] 2) Take it out and continue to stir and impregnate at 30°C until the solvent evaporates completely, forming a solid block.

[0052] 3) Crush the block obtained in step 2, place it in a 40°C oven to dry and keep it at this temperature for 24-48 hours;

[0053] 4) Grinding the produc...

Embodiment 3

[0057] Preparation of palladium / carbon nanotube catalysts with palladium nanoparticles loaded outside the lumen of carbon tubes

[0058] 1) Weigh 1.0g of dry functionalized carbon nanotube support (average inner diameter 5-10nm, outer diameter 10-20nm) into a 50mL round bottom flask, add 20g (about 23.3mL) xylene under stirring, Then place it in an ultrasonic machine for ultrasonic treatment for 2-4 hours;

[0059] 2) Weigh palladium chloride (83.3 mg, palladium content ≥ 60%, 5% palladium loading), add 3 mL of acetone, then add 30 μL of concentrated hydrochloric acid with a mass fraction of 37% to help dissolve the palladium chloride, shake for 3 minutes Allow palladium chloride to dissolve evenly.

[0060] 3) Add 3 mL of the palladium chloride acetone solution in step 2 to the material obtained in step 1 under magnetic stirring, and continue stirring for 15 to 30 minutes after the addition;

[0061] 4) Add 10.0 mL of sodium formate aqueous solution (79.9 mg / mL) to the mixt...

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Abstract

The invention relates to a palladium / carbon nanotube catalyst used for selectively supporting palladium nanoparticles in carbon nanotube chamber or outside the nanotube chamber in alpha, beta unsaturated carboxylic acid hydrogenation reaction, which takes carbon nanotube as a carrier, the palladium nanoparticles can be selectively dispersed in the carbon nanotube chamber or outside the nanotube chamber, the size is uniform, and the particle size is 2-5nm. The catalyst can be used for hydrogenation and asymmetric hydrogenation of asymmetric carboxylic acid. The catalyst appears higher activity than that of the commercialized palladium catalysts in an alpha-phenylcinnamic acid hydrogenation reaction, and the highest reaction activity can reach 564mmol h<-1> g<-1>. When a chiral modification agent cinchonidine and an auxiliary agent benzylamine are added in a reaction system, the enantiomer selectivity of alpha-phenylcinnamic acid asymmetric hydrogenation product can reach more than 75%, the activity is increased to 133mmol h<-1> g<-1>, which is the highest intrinsic reaction activity of a heterogeneous catalyst to the asymmetric hydrogenation reaction of alpha-phenylcinnamic acid.

Description

technical field [0001] The invention relates to a palladium / carbon nanotube catalyst suitable for heterogeneous hydrogenation reactions; [0002] The present invention also relates to the preparation method of above-mentioned palladium / carbon nanotube catalyst; [0003] The present invention also relates to the application of the above-mentioned palladium / carbon nanotube catalyst. Background technique [0004] The continuous development of asymmetric catalysis has made single enantiomer chiral compounds widely used in the fields of fine chemicals such as medicine and pesticides. Taking the pharmaceutical market as an example, in 2009, the global single enantiomer drug production value was close to 15 billion US dollars. Asymmetric catalysis includes homogeneous asymmetric catalysis and heterogeneous asymmetric catalysis. Due to its advantages in product separation and easy industrialization, heterogeneous asymmetric catalysis has always been a method that people focus on ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07B53/00C07C51/36C07C57/38C07C59/64
Inventor 李灿管再鸿卢胜梅
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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