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Oxide supported palladium hydrogenation catalyst and preparation method thereof

A hydrogenation catalyst and oxide technology, applied in catalyst activation/preparation, carbon-based compound preparation, organic compound preparation, etc., can solve problems affecting catalyst performance, etc., and achieve high catalytic activity and selectivity, and the effect of uniform size

Inactive Publication Date: 2011-06-01
葛昌华 +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For example, in Al 2 o 3 During the process of carrying metal cobalt on the carrier, cobalt ions will migrate to Al 2 o 3 Compounds are formed in the crystal lattice, which in turn affects the performance of the catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Weigh a certain amount of zirconium nitrate and dissolve it in deionized water, then slowly add a certain amount of citric acid solution dropwise to form a colorless transparent gel; heat to evaporate the water in the gel until the gel turns into a brown viscous liquid, Dry at 110°C, and bake at 500°C for 2 hours in an air atmosphere to obtain a zirconia carrier.

[0013] Use a pipette to pipette 0.5 mL of chloropalladium acid aqueous solution with a concentration of 0.05 mol / L into a 100 mL three-necked bottle, then add 30 mL of deionized water, add 330 mg of zirconium dioxide under magnetic stirring, and ultrasonically disperse for 1 hour to make Zirconium dioxide is evenly dispersed. Then, under the action of magnetic stirring, 10 mL of potassium borohydride solution with a concentration of 0.005 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 nan...

Embodiment 2

[0015] Take a certain amount of titanium tetrachloride in a beaker, slowly add distilled water dropwise and stir continuously with a glass rod until the liquid is light yellow transparent viscous, add ammonia water dropwise and continue stirring until the pH value is about 10. Filter and wash repeatedly until there is no Cl - exist. Dry at 100°C, and calcinate at 400°C for 2h in an air atmosphere to obtain a titanium dioxide carrier.

[0016] Use a pipette to pipette 0.5 mL of 0.05 mol / L chloropalladium acid aqueous solution into a 100 mL three-necked bottle, then add 30 mL of deionized water, add 330 mg of titanium dioxide under the action of magnetic stirring, and ultrasonically disperse for 1 hour to disperse the titanium dioxide. uniform. Then, under the action of magnetic stirring, 10 mL of potassium borohydride solution with a concentration of 0.005 mol / L was added dropwise, and stirring was continued for 1.5 h after the dropwise addition, so that the chloropalladium a...

Embodiment 3

[0018] A certain amount of aluminum nitrate was weighed and dissolved in water, and ammonia water was added dropwise with stirring until the pH was 9, and after stirring for half an hour, the aluminum oxide wet gel was obtained by aging at room temperature. The obtained wet gel was washed with distilled water, and the water in the gel was replaced with absolute ethanol, dried at 100°C, and calcined at 500°C for 2 hours in an air atmosphere to obtain an aluminum oxide carrier.

[0019] Use a pipette to pipette 0.5 mL of chloropalladium acid aqueous solution with a concentration of 0.05 mol / L and add it to a 100 mL three-necked bottle, then add 30 mL of deionized water, add 330 mg of aluminum oxide under the action of magnetic stirring, and ultrasonically disperse for 1 hour. Make the aluminum oxide dispersed evenly. Then, under the action of magnetic stirring, 10 mL of potassium borohydride solution with a concentration of 0.005 mol / L was added dropwise, and stirring was contin...

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Abstract

The invention discloses an oxide supported palladium hydrogenation catalyst and a preparation method thereof; the catalyst carrier is a metallic oxide; and the active component is noble metal palladium nano particle. The catalyst comprises 0.1-5% palladium and the balance of metallic oxide. The preparation method comprises the following steps: (1) preparing the metallic oxide carrier with sol-gel process; (2) dissolving the palladium salt in the ionized water to prepare the palladium salt water solution of which the concentration is 0.01-0.2 mol / L; adding the metallic oxide in the palladium salt water solution and ultrasonically dispersing for 0.5-1 hour; under the effect of magnetic stirring, adding the water solution containing the reducing agent drop by drop, wherein the ratio of the reducing agent to the palladium salt is (1: 1)-(2: 1); after adding, stirring for 1-2 hours; and (3) stirring in the oil bath for 1-2 hours, then filtering, washing and stoving to obtain the oxide supported palladium hydrogenation catalyst. The oxide supported palladium hydrogenation catalyst has high catalytic activity and high selectivity for the cinnamyl aldehyde hydrogenation to prepare the benzene propanal.

Description

technical field [0001] The invention relates to a catalyst and a preparation method for preparing phenylpropionaldehyde by hydrogenation of cinnamaldehyde, in particular to a preparation method of an oxide-loaded palladium catalyst used to catalyze the hydrogenation of cinnamaldehyde to prepare phenylpropionaldehyde. Background technique [0002] Cinnamaldehyde is a typical α, β-unsaturated aldehyde. The selective catalytic hydrogenation of cinnamaldehyde to cinnamyl alcohol has high industrial value, and the selective catalytic hydrogenation of cinnamaldehyde to phenylpropionaldehyde is also of great value in industrial and biological applications, and is a thermodynamic priority reaction, C=C double The bond energy of the bond is 615KJ·mol -1 , while the bond energy of the C=O double bond is 715KJ·mol -1 , C=C double bond hydrogenation is easier to C=O double bond. In recent years, it has been found that phenylpropanal is an important intermediate of anti-AIDS drugs. I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44B01J37/16C07C47/228C07C45/62
Inventor 葛昌华赵杰李艳周仁贤
Owner 葛昌华
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