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Palladium-charcoal catalyst as well as preparation method and application thereof

A palladium-carbon catalyst and a catalyst technology, which are applied in the directions of catalyst activation/preparation, hydrogenation preparation, chemical instruments and methods, etc., can solve the problems of low utilization rate of palladium atoms, loss of palladium metal, poor catalyst stability, etc., and avoid the recovery of palladium metal. Problems, blocking migration and shedding, effects of high conversion and yield

Active Publication Date: 2019-12-20
ZHEJIANG NHU CO LTD +4
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the reduction process of chemical reducing agents, palladium nanoparticles tend to aggregate, and the agglomeration phenomenon is more serious, which affects its catalytic activity; the agglomerated palladium nanoparticles are very easy to detach, and the stability is poor, resulting in the loss of precious metal palladium; the formed palladium nanoparticles are basically Surrounded by Pd(111) crystal face, its crystal face is single, and its catalytic performance is poor
In the preparation of electrochemical plating deposition, the formation of palladium metal crystals includes the migration and reduction of metal ions, the nucleation of metal atoms, and the growth of nuclei. The migrated metal ions will be reduced to the nucleated metal atoms, resulting in the formation of The palladium metal atoms in the core grow up and aggregate to form large-sized granular nanoparticles, so that most of the atoms are wrapped inside the nanoparticles, making the utilization rate of metal atoms low, and the contact area between the granular nanoparticles and the carrier is small, which is easy to cause Shedding of nanoparticles, resulting in poor catalyst stability and loss of palladium metal
[0004] In addition, traditional palladium-carbon catalysts will inevitably introduce or generate other substances during the preparation process, which will cause the separation and recovery of reaction products and additives or by-products, especially palladium metal is an expensive noble metal, which will cause cost. Increase
[0005] In summary, the preparation method of traditional palladium-carbon catalysts is relatively complicated, and it faces the problems of easy agglomeration, easy falling off, poor stability, low utilization rate of palladium atoms, poor catalytic activity and difficult recovery.

Method used

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  • Palladium-charcoal catalyst as well as preparation method and application thereof
  • Palladium-charcoal catalyst as well as preparation method and application thereof
  • Palladium-charcoal catalyst as well as preparation method and application thereof

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preparation example Construction

[0044] The invention provides a preparation method of palladium carbon catalyst. The preparation method comprises the following steps:

[0045] S1, pretreating the carrier;

[0046] S2. Immersing the carrier in the palladium metal precursor solution, washing and drying to obtain the catalyst precursor;

[0047] S3. Carrying out electrochemical in-situ reduction on the catalyst precursor, so that the palladium ions are reduced to metal palladium to prepare a palladium-carbon catalyst.

[0048] In the above step S1, the carrier in the pretreatment of the carrier includes at least one of activated carbon, carbon nanotubes, carbon fibers, and nitrogen-doped hierarchical porous carbon. Compared with ordinary carbon materials, nitrogen-doped carbon materials have Some unique advantages, such as nitrogen doping can change the local electronic structure of carbon materials, facilitate the dispersion of noble metal nanoparticles, and improve the activity and stability of catalysts th...

Embodiment 1

[0109] Weigh 1g of carbon nanotubes, first acid-treat the carbon nanotubes, put the carbon nanotubes into 50mL of 1mol / L H 2 SO 4 solution, and heated to reflux at 80° C. for 8 hours, and filtered to obtain a black powder after cooling down to room temperature. The black powder was washed with deionized water several times until the aqueous solution became neutral. Then the carbon nanotubes are heat-treated, the black powder is placed in an atmosphere of high-purity nitrogen, and calcined at a temperature of 1000° C. for 2 hours.

[0110] Weigh 0.5g of treated carbon nanotubes into 20mL of deionized water, sonicate for 1 hour, measure and add 0.05mL of PdCl 2 Solution (palladium concentration is 0.05g / mL), ultrasonication for 1 hour; centrifugation, remove the solution, add 20mL deionized water to wash, centrifuge, repeat 5 times, collect black powder, vacuum freeze-dry for 12 hours to obtain the catalyst precursor. Under the three-electrode system with the electrolyte of 1m...

Embodiment 2

[0112] This embodiment is basically the same as embodiment 1, the only difference is: measure 0.1mL of PdCl 2 Solution (palladium concentration is 0.05g / mL), prepares palladium carbon catalyst B, and its palladium loading is 1%.

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Abstract

The invention provides a preparation method of a palladium-charcoal catalyst and further provides the palladium-charcoal catalyst prepared by using the preparation method and application of the palladium-charcoal catalyst. Compared with the prior art, palladium ions which are already adsorbed to a carrier are subjected to in-situ reduction through electrochemical in-situ reduction; compared with aconventional method that a reducing agent is added or electrochemical deposition is implemented, the preparation method is rapid in reduction speed, and the metal palladium takes the shape of sheetsand has a large contact area with the carrier, so that migration and dropping of the palladium metal can be well prevented, and the catalyst is high in stability, high in palladium atom utilization rate and good in catalysis performance; and meanwhile, a high conversion rate and yield can be achieved without adding other metals into the catalyst, and problems of separation and palladium metal recycling caused by conventional preparation methods can be solved.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a palladium-carbon catalyst and its preparation method and application. Background technique [0002] Palladium-based catalyst is a general-purpose catalyst with a wide range of uses and good performance. It has high catalytic activity and selectivity. Hydrogen and catalytic cracking. The palladium carbon catalyst loads the precious metal palladium on the activated carbon, the active palladium is distributed on the surface of the carrier carbon, and the palladium crystals inside help to improve the active agent life of the catalyst. [0003] The preparation of palladium-carbon catalyst generally includes pretreatment of carbon support, impregnation of palladium-containing solution and reduction of palladium. Wherein, the reduction of palladium can be reduced by a chemical reducing agent, or the palladium ions dissociated in the electrolyte can be reduced and deposited by elec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42B01J37/34B01J35/10B01J35/02B82Y30/00B82Y40/00C07C29/17C07C33/14C07C33/03C07C33/02C07C33/035B01J35/00
CPCB01J23/42B01J37/348B82Y30/00B82Y40/00C07C29/17C07C2601/16B01J35/00B01J35/30B01J35/60B01J35/61C07C33/14C07C33/03C07C33/02C07C33/035
Inventor 王勇吕国锋马啸毛善俊王哲于丽丽李建清王柳枫李其川鲍晓冰陈宇卓毛建拥
Owner ZHEJIANG NHU CO LTD
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