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Carbon-carried palladium oxide catalyst, preparation method thereof and application thereof

A palladium oxide and catalyst technology, which is applied in the field of new carbon-supported palladium oxide catalyst and its preparation, can solve the problems of metal active component loss and weak interaction, and achieve the effect of simple preparation method, high dispersion and mild conditions

Active Publication Date: 2013-11-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this organometallic complex has a weak interaction with the carrier, and it is easy to cause the loss of metal active components during the reaction (Explosives, 1996(3), 18-20)

Method used

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  • Carbon-carried palladium oxide catalyst, preparation method thereof and application thereof
  • Carbon-carried palladium oxide catalyst, preparation method thereof and application thereof
  • Carbon-carried palladium oxide catalyst, preparation method thereof and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Pipette 4 mL of chloropalladium acid (H 2 PdCl 4 ) aqueous solution in 20mL deionized water at 10°C, and then slowly add NaOH solution (2wt%) dropwise under stirring to adjust the pH value to 5.0 to obtain a palladium oxide hydrate solution. Another 4.00 g of coconut shell activated carbon and 50 mL of deionized water were prepared into a slurry, and stirred at a constant temperature of 10° C. for half an hour. Then, the above-mentioned palladium oxide hydrate solution was added into the activated carbon slurry, and the stirring was continued at constant temperature for 4 hours. After the impregnation is completed, NaOH solution (2wt%) is added dropwise to adjust the pH value to 8-9. After continuing to stir for half an hour, filter and wash until the filtrate is neutral. According to XPS detection, based on palladium element, the content of divalent palladium in palladium oxide accounts for 83.6%, and palladium accounts for 16.4%.

Embodiment 2

[0034] Pipette 4 mL of palladium chlorate (H 2 PdCl 4 ) aqueous solution in 20mL deionized water at 15°C, and then slowly add NaOH solution (2wt%) dropwise under stirring to adjust the pH value to 5.5 to obtain a palladium oxide hydrate solution. Another 4.00 g of coconut shell activated carbon and 50 mL of deionized water were prepared into a slurry, and stirred at a constant temperature of 15° C. for half an hour. Then, the above-mentioned palladium oxide hydrate solution was added into the activated carbon slurry, and the stirring was continued at constant temperature for 4 hours. After the impregnation is completed, NaOH solution (2wt%) is added dropwise to adjust the pH value to 8-9. After continuing to stir for half an hour, filter and wash until the filtrate is neutral. That is, a carbon-supported palladium oxide catalyst (loading capacity: 5 wt %) was obtained. According to XPS detection, based on palladium element, the content of divalent palladium in palladium ox...

Embodiment 3

[0036] Pipette 4 mL of chloropalladium acid (H 2 PdCl 4) aqueous solution in 20mL deionized water at 20°C, and then slowly add NaOH solution (2wt%) dropwise under stirring to adjust the pH value to 6.0 to obtain a palladium oxide hydrate solution. Another 4.00g of coconut shell activated carbon and 50mL of deionized water were prepared into a slurry, and stirred at a constant temperature of 20°C for half an hour. Then, the above-mentioned palladium oxide hydrate solution was added into the activated carbon slurry, and the stirring was continued at constant temperature for 5 hours. After the impregnation is completed, NaOH solution (2wt%) is added dropwise to adjust the pH value to 8-9. After continuing to stir for half an hour, filter and wash until the filtrate is neutral. That is, a carbon-supported palladium oxide catalyst (loading capacity: 5 wt %) was obtained. According to XPS detection, based on palladium element, the content of divalent palladium in palladium oxide...

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Abstract

The invention discloses a carbon-carried palladium oxide catalyst, a preparation method thereof and an application thereof. The carbon-carried palladium oxide catalyst comprises a carrier, and metal active components carried by the carrier, wherein the metal active components are palladium oxide and palladium elementary substance, the carrier is active carbon, the weight percentage of the palladium element in the catalyst is 0.1-15%, and the weight percentage of bivalent palladium of the palladium oxide in the palladium element is 45-95%. The catalyst can be applied for selective hydrogenation of 1,4-butynediol to synthesize 1,4-butenediol, and shows high catalytic activity and high selectivity.

Description

technical field [0001] The invention relates to a novel carbon-supported palladium oxide catalyst and its preparation method and application. Background technique [0002] Supported palladium catalysts have high catalytic hydrogenation activity and are widely used in chemical production processes such as organic synthesis. However, in selective hydrogenation reactions such as hydrogenation of alkynes to olefins, supported palladium catalysts face selectivity technical difficulties. [0003] 1,4-butenediol can be used to synthesize vitamin VB6, 1,2,4-butanetriol and its derivatives (1,4-butanediol, vinylpyrrolidone, γ-butyrolactone, 2,3-cyclo Oxygen-1,4-butanediol and PBT resin, etc.), are important organic intermediates for synthetic polymer materials, medicine, papermaking, etc. Traditionally, it is prepared by hydrogenation of 1,4-butynediol with Lindlar catalyst. Lindra catalyst is a selective catalytic hydrogenation catalyst consisting of palladium-lead attached to a ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/44C07C33/035C07C29/17
Inventor 卢春山马磊张群峰丰枫梁秋霞李小年
Owner ZHEJIANG UNIV OF TECH
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