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Novel attapulgite supported palladium hydrogenation catalyst and preparation method thereof

A hydrogenation catalyst and attapulgite technology are applied in the field of preparation of attapulgite-supported palladium catalysts, can solve problems such as no reports, and achieve the effects of high selectivity, low cost and small particle size

Inactive Publication Date: 2010-05-26
赵杰 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the application of attapulgite clay in catalysis has received more and more attention in recent years, there has been no research on using it as a carrier to support nano-palladium catalysts and applying it to catalyze the hydrogenation of cinnamaldehyde to prepare phenylpropionaldehyde. to report

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Weigh a certain amount of attapulgite clay into a beaker, add 4mol / L hydrochloric acid at a liquid-solid ratio of 8:1, stir magnetically at room temperature for 12 hours, then centrifuge, wash with distilled water, dry at 105°C, grind and put in a desiccator spare. Use a pipette to pipette 2.0 mL of chloropalladium acid aqueous solution with a concentration of 0.02 mol / L into a 150 mL three-necked bottle, then add 50 mL of deionized water, add 528 mg of acidified attapulgite clay under the action of magnetic stirring, and ultrasonically disperse for 2.5 h , so that the attapulgite is evenly dispersed. Then, under the action of magnetic stirring, 10 mL of potassium borohydride solution with a concentration of 0.008 mol / L was added dropwise, and stirring was continued for 1.5 h after the dropwise addition, so that the chloropalladium acid solution was completely reduced to palladium nanoparticles. Finally, stirring was continued for 2 h in an oil bath at 80 °C until no b...

Embodiment 2

[0020] Weigh a certain amount of attapulgite clay into a beaker, add 2mol / L nitric acid at a liquid-solid ratio of 10:1, stir magnetically at room temperature for 10 hours, then centrifuge, wash with distilled water, dry at 105°C, grind and put in a desiccator spare. Use a pipette to pipette 1.0 mL of chloropalladium acid aqueous solution with a concentration of 0.05 mol / L into a 150 mL three-necked bottle, then add 60 mL of deionized water, add 438 mg of acidified attapulgite clay under magnetic stirring, and ultrasonically disperse for 2 hours. Make the attapulgite disperse evenly. Then, under the action of magnetic stirring, 10 mL of potassium borohydride solution with a concentration of 0.01 mol / L was added dropwise, and stirring was continued for 1.5 h after the dropwise addition, so that the chloropalladium acid solution was completely reduced to palladium nanoparticles. Finally, stirring was continued for 2 h in an oil bath at 80 °C until no bubbles were generated. Th...

Embodiment 3

[0025] Weigh a certain amount of attapulgite clay into a beaker, add 4mol / L hydrochloric acid at a liquid-solid ratio of 10:1, stir magnetically at room temperature for 14 hours, then centrifuge, wash with distilled water, dry at 105°C, grind and put in a desiccator spare. Use a pipette to pipette 1.0 mL of 0.1 mol / L potassium chloropalladate aqueous solution into a 150 mL three-neck flask, then add 80 mL of deionized water, add 344 mg of acidified attapulgite clay under magnetic stirring, and ultrasonically disperse for 2 hours , so that the attapulgite is evenly dispersed. Then, under the action of magnetic stirring, 10 mL of potassium borohydride solution with a concentration of 0.02 mol / L was added dropwise, and stirring was continued for 1.5 h after the dropwise addition, so that the potassium chloropalladate in the solution was completely reduced to palladium nanoparticles. Finally, stirring was continued for 2 h in an oil bath at 80 °C until no bubbles were generated. ...

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Abstract

The invention discloses a novel attapulgite supported palladium hydrogenation catalyst and a preparation method thereof. Acidized attapulgite clay is used as a carrier, potassium borohydride or hydrazine hydrate is used as a reducer, and a soluble palladium salt is reduced to palladium nano particles which are loaded on the acidized attapulgite clay. In the attapulgite loaded palladium hydrogenation catalyst prepared by the method of the invention, the palladium nano particles are fine and uniform and are highly dispersed on the surfaces of carbon nano tubes, and compared with the active carbon or graphite loaded palladium catalyst, the attapulgite loaded palladium hydrogenation catalyst has high activity and selectivity for hydrogenating cinnamyl aldehyde to prepare phenylpropyl aldehyde.

Description

technical field [0001] The present invention relates to a catalyst in the reaction of cinnamaldehyde hydrogenation to prepare phenylpropionaldehyde and a preparation method thereof, in particular to a preparation method of an attapulgite-loaded palladium catalyst used to catalyze the hydrogenation of cinnamaldehyde to prepare phenylpropionaldehyde. Background technique [0002] Cinnamaldehyde is an important α, β-unsaturated aldehyde, and its hydrogenation products cinnamyl alcohol and phenylpropionaldehyde are important intermediates in fine chemicals. Phenylpropionaldehyde is a food flavoring additive. It has recently been found that phenylpropionaldehyde is also an important intermediate for the preparation of anti-AIDS drugs. Therefore, research on the selective catalytic hydrogenation of the C=C bond of cinnamaldehyde has attracted much attention. Since cinnamaldehyde has C=C double bond and C=O double bond at the same time, and is conjugated with the aromatic ring, it ...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J32/00B01J21/16C07C47/228C07C45/62
Inventor 赵杰葛昌华李艳
Owner 赵杰
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